Sample records for uv detection method
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Method for phosphorothioate antisense DNA sequencing by capillary electrophoresis with UV detection.
Froim, D; Hopkins, C E; Belenky, A; Cohen, A S
1997-11-01
The progress of antisense DNA therapy demands development of reliable and convenient methods for sequencing short single-stranded oligonucleotides. A method of phosphorothioate antisense DNA sequencing analysis using UV detection coupled to capillary electrophoresis (CE) has been developed based on a modified chain termination sequencing method. The proposed method reduces the sequencing cost since it uses affordable CE-UV instrumentation and requires no labeling with minimal sample processing before analysis. Cycle sequencing with ThermoSequenase generates quantities of sequencing products that are readily detectable by UV. Discrimination of undesired components from sequencing products in the reaction mixture, previously accomplished by fluorescent or radioactive labeling, is now achieved by bringing concentrations of undesired components below the UV detection range which yields a 'clean', well defined sequence. UV detection coupled with CE offers additional conveniences for sequencing since it can be accomplished with commercially available CE-UV equipment and is readily amenable to automation.
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Method for phosphorothioate antisense DNA sequencing by capillary electrophoresis with UV detection.
Froim, D; Hopkins, C E; Belenky, A; Cohen, A S
1997-01-01
The progress of antisense DNA therapy demands development of reliable and convenient methods for sequencing short single-stranded oligonucleotides. A method of phosphorothioate antisense DNA sequencing analysis using UV detection coupled to capillary electrophoresis (CE) has been developed based on a modified chain termination sequencing method. The proposed method reduces the sequencing cost since it uses affordable CE-UV instrumentation and requires no labeling with minimal sample processing before analysis. Cycle sequencing with ThermoSequenase generates quantities of sequencing products that are readily detectable by UV. Discrimination of undesired components from sequencing products in the reaction mixture, previously accomplished by fluorescent or radioactive labeling, is now achieved by bringing concentrations of undesired components below the UV detection range which yields a 'clean', well defined sequence. UV detection coupled with CE offers additional conveniences for sequencing since it can be accomplished with commercially available CE-UV equipment and is readily amenable to automation. PMID:9336449
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A new passive sampling method with rapid low-cost spectral detection has recently been developed. The method makes use of an ultraviolet (UV)-transparent polymer which serves as both a concentrator for dissolved compounds, and an optical cell for UV spectral detection. Because ...
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Wang, Shu-tao; Wang, Zhi-fang; Liu, Ming-hua; Wei, Meng; Chen, Dong-ying; Wang, Xing-long
2016-01-01
According to the spectral absorption characteristics of polluting gases and fluorescence characteristics, a time-division multiplexing detection system is designed. Through this system we can detect Methane (CH4) and sulfur dioxide (SO2) by using spectral absorption method and the SO2 can be detected by using UV fluorescence method. The system consists of four parts: a combination of a light source which could be switched, the common optical path, the air chamber and the signal processing section. The spectral absorption characteristics and fluorescence characteristics are measured first. Then the experiment of detecting CH4 and SO2 through spectral absorption method and the experiment of detecting SO2 through UV fluorescence method are conducted, respectively. Through measuring characteristics of spectral absorption and fluorescence, we get excitation wavelengths of SO2 and CH4 measured by spectral absorption method at the absorption peak are 280 nm and 1.64 μm, respectively, and the optimal excitation wavelength of SO2 measured by UV fluorescence method is 220 nm. we acquire the linear relation between the concentration of CH4 and relative intensity and the linear relation between the concentration of SO2 and output voltage after conducting the experiment of spectral absorption method, and the linearity are 98.7%, 99.2% respectively. Through the experiment of UV fluorescence method we acquire that the relation between the concentration of SO2 and the voltage is linear, and the linearity is 99.5%. Research shows that the system is able to be applied to detect the polluted gas by absorption spectrum method and UV fluorescence method. Combing these two measurement methods decreases the costing and the volume, and this system can also be used to measure the other gases. Such system has a certain value of application.
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Molecular Viability Testing of UV-Inactivated Bacteria.
Weigel, Kris M; Nguyen, Felicia K; Kearney, Moira R; Meschke, John S; Cangelosi, Gerard A
2017-05-15
PCR is effective in detecting bacterial DNA in samples, but it is unable to differentiate viable bacteria from inactivated cells or free DNA fragments. New PCR-based analytical strategies have been developed to address this limitation. Molecular viability testing (MVT) correlates bacterial viability with the ability to rapidly synthesize species-specific rRNA precursors (pre-rRNA) in response to brief nutritional stimulation. Previous studies demonstrated that MVT can assess bacterial inactivation by chlorine, serum, and low-temperature pasteurization. Here, we demonstrate that MVT can detect inactivation of Escherichia coli , Aeromonas hydrophila , and Enterococcus faecalis cells by UV irradiation. Some UV-inactivated E. coli cells transiently retained the ability to synthesize pre-rRNA postirradiation (generating false-positive MVT results), but this activity ceased within 1 h following UV exposure. Viable but transiently undetectable (by culture) E. coli cells were consistently detected by MVT. An alternative viability testing method, viability PCR (vPCR), correlates viability with cell envelope integrity. This method did not distinguish viable bacteria from UV-inactivated bacteria under some conditions, indicating that the inactivated cells retained intact cell envelopes. MVT holds promise as a means to rapidly assess microbial inactivation by UV treatment. IMPORTANCE UV irradiation is increasingly being used to disinfect water, food, and other materials for human use. Confirming the effectiveness of UV disinfection remains a challenging task. In particular, microbiological methods that rely on rapid detection of microbial DNA can yield misleading results, due to the detection of remnant DNA associated with dead microbial cells. This report describes a novel method that rapidly distinguishes living microbial cells from dead microbial cells after UV disinfection. Copyright © 2017 American Society for Microbiology.
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Shintani, H
1985-05-31
Studies were made of the analytical conditions required for indirect photometric ion chromatography using ultraviolet photometric detection (UV method) for the determination of serum cations following a previously developed serum pre-treatment. The sensitivities of the conductivity detection (CD) and UV methods and the amounts of serum cations determined by both methods were compared. Attempts to improve the sensitivity of the conventional UV method are reported. It was found that the mobile phase previously reported by Small and Miller showed no quantitative response when more than 4 mM copper(II) sulphate pentahydrate was used. As a result, there was no significant difference in the amounts of serum cations shown by the CD and UV methods. However, by adding 0.5-5 mM cobalt(II) sulphate heptahydrate, nickel(II) sulphate hexahydrate, zinc(II) sulphate heptahydrate or cobalt(II) diammonium sulphate hexahydrate to 0.5-1.5 mM copper(II) sulphate pentahydrate, higher sensitivity and a quantitative response were attained.
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A method for the detection of trace levels of N,N-diethyl-m-toluamide (DEET) in water is discussed. The method utilizes an on-line preconcentration column in series with high performance liquid chromatography (HPLC) and UV photodiode array detection. DEET, a common insect repel...
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Peng, Xianzhi; Jin, Jiabin; Wang, Chunwei; Ou, Weihui; Tang, Caiming
2015-03-06
A sensitive and reliable method was developed for multi-target determination of 13 most widely used organic ultraviolet (UV) absorbents (including UV filters and UV stabilizers) in aquatic organism tissues. The organic UV absorbents were extracted using ultrasonic-assisted extraction, purified via gel permeation chromatography coupled with silica gel column chromatography, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry. Recoveries of the UV absorbents from organism tissues mostly ranged from 70% to 120% from fish filet with satisfactory reproducibility. Method quantification limits were 0.003-1.0ngg(-1) dry weight (dw) except for 2-ethylhexyl 4-methoxycinnamate. This method has been applied to analysis of the UV absorbents in wild and farmed aquatic organisms collected from the Pearl River Estuary, South China. 2-Hydroxy-4-methoxybenzophenone and UV-P were frequently detected in both wild and farmed marine organisms at low ngg(-1)dw. 3-(4-Methylbenzylidene)camphor and most of the benzotriazole UV stabilizers were also frequently detected in maricultured fish. Octocrylene and 2-ethylhexyl 4-methoxycinnamate were not detected in any sample. This work lays basis for in-depth study about bioaccumulation and biomagnification of the UV absorbents in marine environment. Copyright © 2015 Elsevier B.V. All rights reserved.
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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.
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Highly Sensitive Detection of UV Radiation Using a Uranium Coordination Polymer.
Liu, Wei; Dai, Xing; Xie, Jian; Silver, Mark A; Zhang, Duo; Wang, Yanlong; Cai, Yawen; Diwu, Juan; Wang, Jian; Zhou, Ruhong; Chai, Zhifang; Wang, Shuao
2018-02-07
The accurate detection of UV radiation is required in a wide range of chemical industries and environmental or biological related applications. Conventional methods taking advantage of semiconductor photodetectors suffer from several drawbacks such as sophisticated synthesis and manufacturing procedure, not being able to measure the accumulated UV dosage as well as high defect density in the material. Searching for new strategies or materials serving as precise UV dosage sensor with extremely low detection limit is still highly desirable. In this work, a radiation resistant uranium coordination polymer [UO 2 (L)(DMF)] (L = 5-nitroisophthalic acid, DMF = N,N-dimethylformamide, denoted as compound 1) was successfully synthesized through mild solvothermal method and investigated as a unique UV probe with the detection limit of 2.4 × 10 -7 J. On the basis of the UV dosage dependent luminescence spectra, EPR analysis, single crystal structure investigation, and the DFT calculation, the UV-induced radical quenching mechanism was confirmed. Importantly, the generated radicals are of significant stability which offers the opportunity for measuring the accumulated UV radiation dosage. Furthermore, the powder material of compound 1 was further upgraded into membrane material without loss in luminescence intensity to investigate the real application potentials. To the best of our knowledge, compound 1 represents the most sensitive coordination polymer based UV dosage probe reported to date.
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Whitehead, Kathryn A; Smith, Lindsay A; Verran, Joanna
2008-09-30
Open food contact surfaces were subjected to organic soiling to provide a source for transfer of microbial cells. Rapid industrial methods used for the detection of residual cells and soil e.g. ATP (adenosine triphosphate) bioluminescence and an ultraviolet (UV) light detection method were assessed for their ability to detect organic soils, or organic soil-cell mix on surfaces. A range of soils (complex [meat extract, fish extract, cottage cheese extract]; oils [cholesterol, fish oil, mixed fatty acids]; proteins [bovine serum albumin, fish peptones casein]; carbohydrates [glycogen, starch, lactose]); was used. Under UV, oily soils, mixed fatty acids, cholesterol and casein were detected at low concentrations, with detection levels ranging from 1% to 0.001% for different substances. Glycogen was the most difficult substance to detect at lower concentrations. Using UV wavelength bands (lambda) of 330-380 nm, 510-560 nm and 590-650 nm, wavelength bands of 330-380 nm, illuminated most of the soils well, whilst the wavelength band of 510-560 nm illuminated the fish extract, cholesterol and fatty acids; the 590-650 nm wavelength band illuminated the lactose. Soils at all concentrations were detected by the ATP bioluminescence method; the complex soils gave the highest readings. When complex soils were combined with Listeria monocytogenes Scott A or a non-pathogenic Escherichia coli O157:H7, ATP measurements increased by 1-2 logs. For UV illumination, the L. monocytogenes and cheese combination was the most intensely illuminated, with E. coli and meat the least. UV illumination is a simple well established method for detecting food soil, with little change in findings when microorganisms are included. Performance can be enhanced in certain circumstances by altering the wavelength. ATP bioluminescence is a proven system for hygienic assessment being especially useful in the presence of microorganisms rather than organic soil alone.
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Qiu, Jun; Wang, Jinhao; Xu, Zhongqi; Liu, Huiqing; Ren, Jie
2017-01-01
The branched-chain amino acids (BCAAs) including leucine (Leu), isoleucine (Ile) and valine (Val) play a pivotal role in the human body. Herein, we developed capillary electrophoresis (CE) coupled with conventional UV detector to quantify underivatized BCAAs in two kinds of sport nutritional supplements. For direct UV detection at 195 nm, the BCAAs (Leu, two enantiomers of Ile and Val) were separated in a background electrolyte (BGE) consisting of 40.0 mmol/L sodium tetraborate, and 40.0 mmol/L β-cyclodextrin (β-CD) at pH 10.2. In addition, the indirect UV detection at 264 nm was achieved in a BGE of 2.0 mmol/L Na2HPO4, 10.0 mmol/L p-aminosalicylic acid (PAS) as UV absorbing probe, and 40.0 mmol/L β-CD at pH 12.2. The β-CD significantly benefited the isomeric separation of Leu, L- and D-Ile. The optimal conditions allowed the LODs (limit of detections) of direct and indirect UV absorption detection to be tens μmol/L level, which was comparable to the reported CE inline derivatization method. The RSDs (relative standard deviations) of migration time and peak area were less than 0.91% and 3.66% (n = 6). Finally, CE with indirect UV detection method was applied for the quantitation of BCAAs in two commercial sport nutritional supplements, and good recovery and precision were obtained. Such simple CE method without tedious derivatization process is feasible of quality control and efficacy evaluation of the supplemental proteins.
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Liu, Huiqing; Ren, Jie
2017-01-01
The branched-chain amino acids (BCAAs) including leucine (Leu), isoleucine (Ile) and valine (Val) play a pivotal role in the human body. Herein, we developed capillary electrophoresis (CE) coupled with conventional UV detector to quantify underivatized BCAAs in two kinds of sport nutritional supplements. For direct UV detection at 195 nm, the BCAAs (Leu, two enantiomers of Ile and Val) were separated in a background electrolyte (BGE) consisting of 40.0 mmol/L sodium tetraborate, and 40.0 mmol/L β-cyclodextrin (β-CD) at pH 10.2. In addition, the indirect UV detection at 264 nm was achieved in a BGE of 2.0 mmol/L Na2HPO4, 10.0 mmol/L p-aminosalicylic acid (PAS) as UV absorbing probe, and 40.0 mmol/L β-CD at pH 12.2. The β-CD significantly benefited the isomeric separation of Leu, L- and D-Ile. The optimal conditions allowed the LODs (limit of detections) of direct and indirect UV absorption detection to be tens μmol/L level, which was comparable to the reported CE inline derivatization method. The RSDs (relative standard deviations) of migration time and peak area were less than 0.91% and 3.66% (n = 6). Finally, CE with indirect UV detection method was applied for the quantitation of BCAAs in two commercial sport nutritional supplements, and good recovery and precision were obtained. Such simple CE method without tedious derivatization process is feasible of quality control and efficacy evaluation of the supplemental proteins. PMID:28640882
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Liu, Yong-Qiang; Yu, Hong
2017-04-01
A convenient and versatile method was developed for the separation and detection of alkaline earth metal ions by ion chromatography with indirect UV detection. The chromatographic separation of Mg 2+ , Ca 2+ , and Sr 2+ was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid as the mobile phase, in which the imidazolium ionic liquid acted as an UV-absorption reagent. The effects of imidazolium ionic liquids, detection wavelength, acids in the mobile phase, and column temperature on the retention of Mg 2+ , Ca 2+ , and Sr 2+ were investigated. The main factors influencing the separation and detection were the background UV absorption reagent and the concentration of hydrogen ion in ion chromatography with indirect UV detection. The successful separation and detection of Mg 2+ , Ca 2+ , and Sr 2+ within 14 min were achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.06, 0.12, and 0.23 mg/L, respectively. A new separation and detection method of alkaline earth metal ions by ion chromatography with indirect UV detection was developed, and the application range of ionic liquids was expanded. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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76 FR 38033 - Cloquintocet-mexyl; Pesticide Tolerances
Federal Register 2010, 2011, 2012, 2013, 2014
2011-06-29
... enforcement methods are the High Performance Liquid Chromatography with Ultraviolet Detection (HPLC/UV) method REM 138.01 for determination of cloquintocet-mexyl (parent) and the HPLC/UV Method REM 138.10 for...
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Geissler, David; Belder, Detlev
2015-12-01
One of the most commonly employed detection methods in microfluidic research is fluorescence detection, due to its ease of integration and excellent sensitivity. Many analytes though do not show luminescence when excited in the visible light spectrum, require suitable dyes. Deep-ultraviolet (UV) excitation (<300 nm) allows label-free detection of a broader range of analytes but also mandates the use of expensive fused silica glass, which is transparent to UV light. Herein, we report the first application of label-free deep UV fluorescence detection in non-UV transparent full-body polymer microfluidic devices. This was achieved by means of two-photon excitation in the visible range (λex = 532 nm). Issues associated with the low optical transmittance of plastics in the UV range were successfully circumvented in this way. The technique was investigated by application to microchip electrophoresis of small aromatic compounds. Various polymers, such as poly(methyl methacrylate), cyclic olefin polymer, and copolymer as well as poly(dimethylsiloxane) were investigated and compared with respect to achievable LOD and ruggedness against photodamage. To demonstrate the applicability of the technique, the method was also applied to the determination of serotonin and tryptamine in fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Zhang, Kelly; Li, Yi; Tsang, Midco; Chetwyn, Nik P
2013-09-01
To overcome challenges in HPLC impurity analysis of pharmaceuticals, we developed an automated online multi-heartcutting 2D HPLC system with hyphenated UV-charged aerosol MS detection. The first dimension has a primary column and the second dimension has six orthogonal columns to enhance flexibility and selectivity. The two dimensions were interfaced by a pair of switching valves equipped with six trapping loops that allow multi-heartcutting of peaks of interest in the first dimension and also allow "peak parking." The hyphenated UV-charged aerosol MS detection provides comprehensive detection for compounds with and without UV chromophores, organics, and inorganics. It also provides structural information for impurity identification. A hidden degradation product that co-eluted with the drug main peak was revealed by RP × RP separation and thus enabled the stability-indicating method development. A poorly retained polar component with no UV chromophores was analyzed by RP × hydrophilic interaction liquid chromatography separation with charged aerosol detection. Furthermore, using this system, the structures of low-level impurities separated by a method using nonvolatile phosphate buffer were identified and tracked by MS in the second dimension. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Myatt, Theodore A; Johnston, Sebastian L; Rudnick, Stephen; Milton, Donald K
2003-01-01
Background Rhinovirus, the most common cause of upper respiratory tract infections, has been implicated in asthma exacerbations and possibly asthma deaths. Although the method of transmission of rhinoviruses is disputed, several studies have demonstrated that aerosol transmission is a likely method of transmission among adults. As a first step in studies of possible airborne rhinovirus transmission, we developed methods to detect aerosolized rhinovirus by extending existing technology for detecting infectious agents in nasal specimens. Methods We aerosolized rhinovirus in a small aerosol chamber. Experiments were conducted with decreasing concentrations of rhinovirus. To determine the effect of UV irradiation on detection of rhinoviral aerosols, we also conducted experiments in which we exposed aerosols to a UV dose of 684 mJ/m2. Aerosols were collected on Teflon filters and rhinovirus recovered in Qiagen AVL buffer using the Qiagen QIAamp Viral RNA Kit (Qiagen Corp., Valencia, California) followed by semi-nested RT-PCR and detection by gel electrophoresis. Results We obtained positive results from filter samples that had collected at least 1.3 TCID50 of aerosolized rhinovirus. Ultraviolet irradiation of airborne virus at doses much greater than those used in upper-room UV germicidal irradiation applications did not inhibit subsequent detection with the RT-PCR assay. Conclusion The air sampling and extraction methodology developed in this study should be applicable to the detection of rhinovirus and other airborne viruses in the indoor air of offices and schools. This method, however, cannot distinguish UV inactivated virus from infectious viral particles. PMID:12525263
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Mazumder, Avik; Gupta, Hemendra K; Garg, Prabhat; Jain, Rajeev; Dubey, Devendra K
2009-07-03
This paper details an on-flow liquid chromatography-ultraviolet-nuclear magnetic resonance (LC-UV-NMR) method for the retrospective detection and identification of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the markers of the toxic nerve agents for verification of the Chemical Weapons Convention (CWC). Initially, the LC-UV-NMR parameters were optimized for benzyl derivatives of the APAs and AAPAs. The optimized parameters include stationary phase C(18), mobile phase methanol:water 78:22 (v/v), UV detection at 268nm and (1)H NMR acquisition conditions. The protocol described herein allowed the detection of analytes through acquisition of high quality NMR spectra from the aqueous solution of the APAs and AAPAs with high concentrations of interfering background chemicals which have been removed by preceding sample preparation. The reported standard deviation for the quantification is related to the UV detector which showed relative standard deviations (RSDs) for quantification within +/-1.1%, while lower limit of detection upto 16mug (in mug absolute) for the NMR detector. Finally the developed LC-UV-NMR method was applied to identify the APAs and AAPAs in real water samples, consequent to solid phase extraction and derivatization. The method is fast (total experiment time approximately 2h), sensitive, rugged and efficient.
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Shimizu, Hisashi; Miyawaki, Naoya; Asano, Yoshihiro; Mawatari, Kazuma; Kitamori, Takehiko
2017-06-06
The expansion of microfluidics research to nanofluidics requires absolutely sensitive and universal detection methods. Photothermal detection, which utilizes optical absorption and nonradiative relaxation, is promising for the sensitive detection of nonlabeled biomolecules in nanofluidic channels. We have previously developed a photothermal optical phase shift (POPS) detection method to detect nonfluorescent molecules sensitively, while a rapid decrease of the sensitivity in nanochannels and the introduction of an ultraviolet (UV) excitation system were issues to be addressed. In the present study, our primary aim is to characterize the POPS signal in terms of the thermo-optical properties and quantitatively evaluate the causes for the decrease in sensitivity. The UV excitation system is then introduced into the POPS detector to realize the sensitive detection of nonlabeled biomolecules. The UV-POPS detection system is designed and constructed from scratch based on a symmetric microscope. The results of simulations and experiments reveal that the sensitivity decreases due to a reduction of the detection volume, dissipation of the heat, and cancellation of the changes in the refractive indices. Finally, determination of the concentration of a nonlabeled protein (bovine serum albumin) is performed in a very thin 900 nm deep nanochannel. As a result, the limit of detection (LOD) is 2.3 μM (600 molecules in the 440 attoliter detection volume), which is as low as that previously obtained for our visible POPS detector. UV-POPS detection is thus expected be a powerful technique for the study of biomolecules, including DNAs and proteins confined in nanofluidic channels.
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Mustafaoglu, Nur; Alves, Nathan J; Bilgicer, Basar
2015-09-08
Oriented immobilization of antibodies and antibody fragments has become increasingly important as a result of the efforts to reduce the size of diagnostic and sensor devices to miniaturized dimensions for improved accessibility to the end-user. Reduced dimensions of sensor devices necessitate the immobilized antibodies to conserve their antigen binding activity for proper operation. Fab fragments are becoming more commonly used in small-scaled diagnostic devices due to their small size and ease of manufacture. In this study, we used the previously described UV-NBS(Biotin) method to functionalize Fab fragments with IBA-EG11-Biotin linker utilizing UV energy to initiate a photo-cross-linking reaction between the nucleotide binding site (NBS) on the Fab fragment and IBA-Biotin molecule. Our results demonstrate that immobilization of biotinylated Fab fragments via UV-NBS(Biotin) method generated the highest level of immobilized Fab on surfaces when compared to other typical immobilization methods while preserving antigen binding activity. UV-NBS(Biotin) method provided 432-fold, 114-fold, and 29-fold improved antigen detection sensitivity than physical adsorption, NHS-Biotin, and ε-NH3(+), methods, respectively. Additionally, the limit of detection (LOD) for PSA utilizing Fab fragments immobilized via UV-NBS(Biotin) method was significantly lower than that of the other immobilization methods, with an LOD of 0.4 pM PSA. In summary, site-specific biotinylation of Fab fragments without structural damage or loss in antigen binding activity provides a wide range of application potential for UV-NBS immobilization technique across numerous diagnostic devices and nanotechnologies.
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da Costa César, Isabela; Nogueira, Fernando Henrique Andrade; Pianetti, Gérson Antônio
2008-09-10
This paper describes the development and evaluation of a HPLC, UV spectrophotometry and potentiometric titration methods to quantify lumefantrine in raw materials and tablets. HPLC analyses were carried out using a Symmetry C(18) column and a mobile phase composed of methanol and 0.05% trifluoroacetic acid (80:20), with a flow rate of 1.0ml/min and UV detection at 335nm. For the spectrophotometric analyses, methanol was used as solvent and the wavelength of 335nm was selected for the detection. Non-aqueous titration of lumefantrine was carried out using perchloric acid as titrant and glacial acetic acid/acetic anhydride as solvent. The end point was potentiometrically determined. The three evaluated methods showed to be adequate to quantify lumefantrine in raw materials, while HPLC and UV methods presented the most reliable results for the analyses of tablets.
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USDA-ARS?s Scientific Manuscript database
Fecal contamination of produce is a known food safety risk. Measuring fluorescence responses to UV excitation is an established method for detecting such contamination. One measurement system utilizes a pulsed UV laser to induce a fluorescence response from fecal material and a gated intensified cam...
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Tessem, May-Britt; Bathen, Tone F; Cejková, Jitka; Midelfart, Anna
2005-03-01
This study was conducted to investigate metabolic changes in aqueous humor from rabbit eyes exposed to either UV-A or -B radiation, by using (1)H nuclear magnetic resonance (NMR) spectroscopy and unsupervised pattern recognition methods. Both eyes of adult albino rabbits were irradiated with UV-A (366 nm, 0.589 J/cm(2)) or UV-B (312 nm, 1.667 J/cm(2)) radiation for 8 minutes, once a day for 5 days. Three days after the last irradiation, samples of aqueous humor were aspirated, and the metabolic profiles analyzed with (1)H NMR spectroscopy. The metabolic concentrations in the exposed and control materials were statistically analyzed and compared, with multivariate methods and one-way ANOVA. UV-B radiation caused statistically significant alterations of betaine, glucose, ascorbate, valine, isoleucine, and formate in the rabbit aqueous humor. By using principal component analysis, the UV-B-irradiated samples were clearly separated from the UV-A-irradiated samples and the control group. No significant metabolic changes were detected in UV-A-irradiated samples. This study demonstrates the potential of using unsupervised pattern recognition methods to extract valuable metabolic information from complex (1)H NMR spectra. UV-B irradiation of rabbit eyes led to significant metabolic changes in the aqueous humor detected 3 days after the last exposure.
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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.
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Detection of UV Pulse from Insulators and Application in Estimating the Conditions of Insulators
NASA Astrophysics Data System (ADS)
Wang, Jingang; Chong, Junlong; Yang, Jie
2014-10-01
Solar radiation in the band of 240-280 nm is absorbed by the ozone layer in the atmosphere, and corona discharges from high-voltage apparatus emit in air mainly in the 230-405 nm range of ultraviolet (UV), so the band of 240-280 nm is called UV Solar Blind Band. When the insulators in a string deteriorate or are contaminated, the voltage distribution along the string will change, which causes the electric fields in the vicinity of insulators change and corona discharge intensifies. An UV pulse detection method to check the conditions of insulators is presented based on detecting the UV pulse among the corona discharge, then it can be confirmed that whether there exist faulty insulators and whether the surface contamination of insulators is severe for the safe operation of power systems. An UV-I Insulator Detector has been developed, and both laboratory tests and field tests have been carried out which demonstrates the practical viability of UV-I Insulator Detector for online monitoring.
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Srinubabu, Gedela; Sudharani, Batchu; Sridhar, Lade; Rao, Jvln Seshagiri
2006-06-01
A high-performance liquid chromatographic method and a UV derivative spectrophotometric method for the determination of famciclovir, a highly active antiviral agent, in tablets were developed in the present work. The various parameters, such as linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. HPLC was carried out by using the reversed-phase technique on an RP-18 column with a mobile phase composed of 50 mM monobasic phosphate buffer and methanol (50 : 50; v/v), adjusted to pH 3.05 with orthophosphoric acid. The mobile phase was pumped at a flow rate of 1 ml/min and detection was made at 242 nm with UV dual absorbance detector. The first derivative UV spectrophotometric method was performed at 226.5 nm. Statistical analysis was done by Student's t-test and F-test, which showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and therefore can be used for its Intended purpose.
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Wada, Mitsuhiro; Inoue, Keiyu; Thara, Ayuko; Kishikawa, Naoya; Nakashima, Kenichiro; Kuroda, Naotaka
2003-02-14
A HPLC method was developed for the simultaneous determination of organic peroxides and hydrogen peroxide with peroxyoxalate chemiluminescence (PO-CL) detection following on-line UV irradiation. Organic peroxides [i.e., benzoyl peroxide (BP), tert.-butyl hydroperoxide (BHP), tert.-butyl perbenzoate (BPB), cumene hydroperoxide (CHP)] were UV irradiated (254 nm, 15 W) to generate hydrogen peroxide, which was determined by PO-CL detection. The conditions for UV irradiation and PO-CL detection were optimized by a flow injection analysis (FIA) system. Generation of hydrogen peroxide from peroxides with on-line UV irradiation also was confirmed by the FIA system by incorporating an enzyme column reactor immobilized with catalase. The separation of four organic peroxides and hydrogen peroxide by HPLC was accomplished isocratically on an ODS column within 30 min. The detection limits (signal-to-noise ratio=3) were 1.1 microM for hydrogen peroxide, 6.8 microM for BP, 31.3 microM for BHP, 7.5 microM for BPB and 1.3 microM for CHP. The proposed method was applied to the determination of BP in wheat flour.
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An estimation methode for measurement of ultraviolet radiation during nondestructive testing
NASA Astrophysics Data System (ADS)
Hosseinipanah, M.; Movafeghi, A.; Farvadin, D.
2018-04-01
Dye penetrant testing and magnetic particle testing are among conventional NDT methods. For increased sensitivity, fluorescence dyes and particles can be used with ultraviolet (black) lights. UV flaw detection lights have different spectra. With the help of photo-filters, the output lights are transferred to UV-A and visible zones. UV-A light can be harmful to human eyes in some conditions. In this research, UV intensity and spectrum were obtained by a Radio-spectrometer for two different UV flaw detector lighting systems. According to the standards such as ASTM E709, UV intensity must be at least 10 W/m2 at a distance of 30 cm. Based on our measurements; these features not achieved in some lamps. On the other hand, intensity and effective intensity of UV lights must be below the some limits for prevention of unprotected eye damage. NDT centers are usually using some type of UV measuring devices. A method for the estimation of effective intensity of UV light has been proposed in this research.
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Park, Ah Yeon; Park, So-Young; Lee, Jaehyun; Jung, Mihye; Kim, Jinwoong; Kang, Sam Sik; Youm, Jeong-Rok; Han, Sang Beom
2009-10-01
Rapid, simple and reliable HPLC/UV and LC-ESI-MS/MS methods for the simultaneous determination of five active coumarins of Angelicae dahuricae Radix, byakangelicol (1), oxypeucedanin (2), imperatorin (3), phellopterin (4) and isoimperatorin (5) were developed and validated. The separation condition for HPLC/UV was optimized using a Develosil RPAQUEOUS C(30) column using 70% acetonitrile in water as the mobile phase. This HPLC/UV method was successful for providing the baseline separation of the five coumarins with no interfering peaks detected in the 70% ethanol extract of Angelicae dahuricae Radix. The specific determination of the five coumarins was also accomplished by a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization source (LC-ESI-MS/MS). Multiple reaction monitoring (MRM) in the positive mode was used to enhance the selectivity of detection. The LC-ESI-MS/MS methods were successfully applied for the determination of the five major coumarins in Angelicae dahuricae Radix. These HPLC/UV and LC-ESI-MS/MS methods were validated in terms of recovery, linearity, accuracy and precision (intra- and inter-day validation). Taken together, the shorter analysis time involved makes these HPLC/UV and LC-ESI-MS/MS methods valuable for the commercial quality control of Angelicae dahuricae Radix extracts and its pharmaceutical preparations. Copyright (c) 2009 John Wiley & Sons, Ltd.
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Sadeghipour, F; Veuthey, J L
1997-11-07
A rapid, sensitive and selective liquid chromatographic method with fluorimetric detection was developed for the separation and quantification of four methylenedioxylated amphetamines without interference of other drugs of abuse and common substances found in illicit tablets. The method was validated by examining linearity, precision and accuracy as well as detection and quantification limits. Methylenedioxylated amphetamines were quantified in eight tablets from illicit drug seizures and results were quantitatively compared to HPLC-UV analyses. To demonstrate the better sensitivity of the fluorimetric detection, methylenedioxylated amphetamines were analyzed in serum after a liquid-liquid extraction procedure and results were also compared to HPLC-UV analyses.
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Improved sensing using simultaneous deep-UV Raman and fluorescence detection-II
NASA Astrophysics Data System (ADS)
Hug, W. F.; Bhartia, R.; Sijapati, K.; Beegle, L. W.; Reid, R. D.
2014-05-01
Photon Systems in collaboration with JPL is continuing development of a new technology robot-mounted or hand-held sensor for reagentless, short-range, standoff detection and identification of trace levels chemical, biological, and explosive (CBE) materials on surfaces. This deep ultraviolet CBE sensor is the result of Army STTR and DTRA programs. The evolving 10 to 15 lb, 20 W, sensor can discriminate CBE from background clutter materials using a fusion of deep UV excited resonance Raman (RR) and laser induced native fluorescence (LINF) emissions collected is less than 1 ms. RR is a method that provides information about molecular bonds, while LINF spectroscopy is a much more sensitive method that provides information regarding the electronic configuration of target molecules. Standoff excitation of suspicious packages, vehicles, persons, and other objects that may contain hazardous materials is accomplished using excitation in the deep UV where there are four main advantages compared to near-UV, visible or near-IR counterparts. 1) Excited between 220 and 250 nm, Raman emission occur within a fluorescence-free region of the spectrum, eliminating obscuration of weak Raman signals by fluorescence from target or surrounding materials. 2) Because Raman and fluorescence occupy separate spectral regions, detection can be done simultaneously, providing an orthogonal set of information to improve both sensitivity and lower false alarm rates. 3) Rayleigh law and resonance effects increase Raman signal strength and sensitivity of detection. 4) Penetration depth into target in the deep UV is short, providing spatial/spectral separation of a target material from its background or substrate. 5) Detection in the deep UV eliminates ambient light background and enable daylight detection.
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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.
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Naked eye detection of mutagenic DNA photodimers using gold nanoparticles.
Kim, Joong Hyun; Chung, Bong Hyun
2011-01-15
We developed a method to detect mutagenic DNA photodimers by the naked eye using gold nanoparticles. The stability of gold nanoparticles in a high ionic strength solution is maintained by straight ssDNA adsorbed physically on the AuNPs. However, we found that UV-irradiated DNA was less adsorptive onto gold nanoparticles because of a conformational change of UV-irradiated DNA. The accumulated deformation of the DNA structure by multiple-dimer formation triggered aggregation of the gold nanoparticles mixed with the UV-irradiated DNA and thus red to purple color changes of the mixture, which allowed colorimetric detection of the DNA photodimers by the naked eye. No fragmented mass and reactive oxygen species production under the UVB irradiation confirmed that the aggregation of gold nanoparticles was solely attributed to the accumulated deformation of the UV irradiated DNA. The degree of gold nanoparticles-aggregation was dependent on the UVB irradiated time and base compositions of the UV-irradiated oligonucleotides. In addition, we successfully demonstrated how to visually qualify the photosensitizing effect of chemical compounds in parallel within only 10 min by applying this new method. Since our method does not require any chemical or biochemical treatments or special instruments for purifying and qualifying the DNA photolesions, it should provide a feasible tool for the studies of the UV-induced mutagenic or carcinogenic DNA dimers and accelerate screening of a large number of drug candidates. Crown Copyright © 2010. Published by Elsevier B.V. All rights reserved.
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Kim, Dalho; Han, Jungho; Choi, Yongwook
2013-01-01
A method using on-line solid-phase microextraction (SPME) on a carbowax-templated fiber followed by liquid chromatography (LC) with ultraviolet (UV) detection was developed for the determination of triclosan in environmental water samples. Along with triclosan, other selected phenolic compounds, bisphenol A, and acidic pharmaceuticals were studied. Previous SPME/LC or stir-bar sorptive extraction/LC-UV for polar analytes showed lack of sensitivity. In this study, the calculated octanol-water distribution coefficient (log D) values of the target analytes at different pH values were used to estimate polarity of the analytes. The lack of sensitivity observed in earlier studies is identified as a lack of desorption by strong polar-polar interactions between analyte and solid-phase. Calculated log D values were useful to understand or predict the interaction between analyte and solid phase. Under the optimized conditions, the method detection limit of selected analytes by using on-line SPME-LC-UV method ranged from 5 to 33 ng L(-1), except for very polar 3-chlorophenol and 2,4-dichlorophenol which was obscured in wastewater samples by an interfering substance. This level of detection represented a remarkable improvement over the conventional existing methods. The on-line SPME-LC-UV method, which did not require derivatization of analytes, was applied to the determination of TCS including phenolic compounds and acidic pharmaceuticals in tap water and river water and municipal wastewater samples.
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Determination of CMPO using HPLC -UV
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gracy Elias; Gary S. Groenewold; Bruce J. Mincher
Octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) is an extractant proposed for selective separation of radionuclide metals from used nuclear fuel solutions using solvent extraction. Radiolysis reactions can degrade CMPO and reduce separation performance and hence methods for measuring concentration of CMPO and identifying degradation products are needed. A novel high performance liquid chromatography (HPLC) method employing ultraviolet detection (UV) was developed to detect and quantitate CMPO in dodecane. Some radiolysis products in gamma and alpha irradiated CMPO solutions were identified using HPLC/electrospray ionization-mass spectrometry (ESI-MS). Validation data indicated that the HPLC-UV method for CMPO determination provided good linearity, sensitivity, procedure accuracy and systemmore » precision. CMPO-nitric acid complexes were also identified, that account for the apparent loss of CMPO in acidic environment, independent of irradiation.« less
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Soni, Hiral; Kothari, Charmy; Khatri, Deepak; Mehta, Priti
2014-01-01
Validated RP-HPLC, HPTLC, and UV spectrophotometric methods have been developed for the simultaneous determination of atorvastatin calcium (ATV) and olmesartan medoxomil (OLM) in a pharmaceutical formulation. The RP-HPLC separation was achieved on a Kromasil C18 column (250 x 4.6 mm, 5 microm particle size) using 0.01 M potassium dihydrogen o-phosphate (pH 4 adjusted with o-phosphoric acid)-acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1.5 mL/min. Quantification was achieved by UV detection at 276 nm. The HPTLC separation was achieved on precoated silica gel 60F254 plates using chloroform-methanol-acetonitrile (4 + 2+ 4, v/v/v) mobile phase. Quantification was achieved with UV detection at 276 nm. The UV-Vis spectrophotometric method was based on the simultaneous equation method that involves measurement of absorbance at two wavelengths, i.e., 255 nm (lambda max of OLM) and 246.2 nm (lambda max of ATV) in methanol. All three methods were validated as per International Conference on Harmonization guidelines. The proposed methods were simple, precise, accurate, and applicable for the simultaneous determination of ATV and OLM in a marketed formulation. The results obtained by applying the proposed methods were statistically analyzed and were found satisfactory.
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Method development and validation of potent pyrimidine derivative by UV-VIS spectrophotometer.
Chaudhary, Anshu; Singh, Anoop; Verma, Prabhakar Kumar
2014-12-01
A rapid and sensitive ultraviolet-visible (UV-VIS) spectroscopic method was developed for the estimation of pyrimidine derivative 6-Bromo-3-(6-(2,6-dichlorophenyl)-2-(morpolinomethylamino) pyrimidine4-yl) -2H-chromen-2-one (BT10M) in bulk form. Pyrimidine derivative was monitored at 275 nm with UV detection, and there is no interference of diluents at 275 nm. The method was found to be linear in the range of 50 to 150 μg/ml. The accuracy and precision were determined and validated statistically. The method was validated as a guideline. The results showed that the proposed method is suitable for the accurate, precise, and rapid determination of pyrimidine derivative. Graphical Abstract Method development and validation of potent pyrimidine derivative by UV spectroscopy.
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Zhao, Xue; Zhang, Zi-Feng; Xu, Lei; Liu, Li-Yan; Song, Wei-Wei; Zhu, Fu-Jie; Li, Yi-Fan; Ma, Wan-Li
2017-08-01
Benzotriazoles (BTs) UV filters are widely used as ultraviolet absorbents for our daily products, which received increasing attention in the past decades. Residential wastewater treatment plant (WWTP) is both an important sink for wastewater and a key pollution source for receiving water for these chemicals. In this study, pretreatment and gas chromatography-tandem mass spectrometry analysis method were developed to determine the occurrence and fate of 9 BTs UV filters in wastewater and sludge from the WWTP with anaerobic-oxic treatment process (A/O) and biological aerated filter treatment process (BAF). Totally, 81 wastewater samples and 11 sludge samples were collected in four seasons. In wastewater, UV-326 and UV-329 were frequently detected, while the highest mean concentrations were detected for UV-234 and UV-329. The concentrations were in the range of
85% in A/O process and 60-77% in BAF process except for UV-350, which was more difficult to remove with lower removal efficiencies of 33.3% for both A/O and BAF. All the target chemicals except for UV-320 were detected in sludge samples with the mean concentration ranging from 0.90 ng/g to 303.39 ng/g. There was no significant difference with concentrations and removal efficiency among different seasons. Higher detection frequency and concentration of BTs UV filters in downstream of the receiving water system indicated the contribution of effluent of the WWTP. Compared with other rivers, the lower concentrations in surface water in the Songhua River indicated light pollution status with of BTs UV filters. Copyright © 2017 Elsevier Ltd. All rights reserved. -
Mustafaoglu, Nur; Alves, Nathan J; Bilgicer, Basar
2015-07-01
The nucleotide binding site (NBS) is a highly conserved region between the variable light and heavy chains at the Fab domains of all antibodies, and a small molecule that we identified, indole-3-butyric acid (IBA), binds specifically to this site. Fab fragment, with its small size and simple production methods compared to intact antibody, is good candidate for use in miniaturized diagnostic devices and targeted therapeutic applications. However, commonly used modification techniques are not well suited for Fab fragments as they are often more delicate than intact antibodies. Fab fragments are of particular interest for sensor surface functionalization but immobilization results in damage to the antigen binding site and greatly reduced activity due to their truncated size that allows only a small area that can bind to surfaces without impeding antigen binding. In this study, we describe an NBS-UV photocrosslinking functionalization method (UV-NBS(Biotin) in which a Fab fragment is site-specifically biotinylated with an IBA-EG11-Biotin linker via UV energy exposure (1 J/cm(2)) without affecting its antigen binding activity. This study demonstrates successful immobilization of biotinylated Ebola detecting Fab fragment (KZ52 Fab fragment) via the UV-NBS(Biotin) method yielding 1031-fold and 2-fold better antigen detection sensitivity compared to commonly used immobilization methods: direct physical adsorption and NHS-Biotin functionalization, respectively. Utilization of the UV-NBS(Biotin) method for site-specific conjugation to Fab fragment represents a proof of concept use of Fab fragment for various diagnostic and therapeutic applications with numerous fluorescent probes, affinity molecules and peptides. © 2015 Wiley Periodicals, Inc.
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USDA-ARS?s Scientific Manuscript database
This study describes the first analytical method for the determination of saponins and alkenated-phenolics from the leaves, leaves/stems and roots of Labisia pumila using a HPLC-UV-ELSD method. The separation was achieved using a reversed phase column, PDA and ELS detection, and a water/acetonitrile...
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USDA-ARS?s Scientific Manuscript database
This study describes the first analytical method for the determination of saponins and alkenated-phenolics from the leaves, leaves/stems and roots of Labisia pumila using a HPLC-UV-ELSD method. The separation was achieved using a reversed phase column, PDA and ELS detection, and a water/acetonitrile...
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van der Heeft, E; Dijkman, E; Baumann, R A; Hogendoorn, E A
2000-05-19
The performance of mass spectrometric (MS) detection and UV detection in combination with reversed-phase liquid chromatography without and with the use of coupled column RPLC (LC-LC) has been compared for the trace analysis of phenylurea herbicides in environmental waters. The selected samples of this comparative study originated from an inter-laboratory study. For both detection modes, a 50 mm x 4.6 mm I.D. column and a 100 mm x 4.6 mm I.D. column packed with 3 microm C18 were used as the first (C-1) and second (C-2) column, respectively. Atmospheric pressure chemical ionization mass spectrometry was performed on a magnetic sector instrument. The LC-LC-MS analysis was carried out on-line by means of direct large volume (11.7 ml) injection (LVI). The performance of both on-line (LVI, 4 ml of sample) and off-line LC-LC-UV (244 nm) analysis was investigated. The latter procedure consisted of a solid-phase extraction (SPE) of 250 ml of water sample on a 500 mg C18 cartridge. The comparative study showed that LC-LC-MS is more selective then LC-LC-UV and, in most cases, more sensitive. The LVI-LC-LC-MS approach combines direct quantification and confirmation of most of the analytes down to a level of 0.01 microg/l in water samples in less then 30 min. As regards LC-LC-UV, the off-line method appeared to be a more viable approach in comparison with the on-line procedure. This method allows the screening of phenylurea's in various types of water samples down to a level of at least 0.05 microg/l. On-line analysis with LVI provided marginal sensitivity (limits of detection of about 0.1 microg/l) and selectivity was sometimes less in case of surface water samples. Both the on-line LVI-LC-LC-MS method and the LC-LC-UV method using off-line SPE were validated by analysing a series of real-life reference samples. These samples were part of an inter-laboratory test and contained residues of herbicides ranging from 0.02 to 0.8 microg/l. Beside good correlation between the methods the data agreed very well with the true values of the samples.
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Filip, Katarzyna; Grynkiewicz, Grzegorz; Gruza, Mariusz; Jatczak, Kamil; Zagrodzki, Bogdan
2014-01-01
Escin, a complex mixture of pentacyclic triterpene saponins obtained from horse chestnut seeds extract (HCSE; Aesculus hippocastanum L.), constitutes a traditional herbal active substance of preparations (drugs) used for a treatment of chronic venous insufficiency and capillary blood vessel leakage. A new approach to exploitation of pharmacological potential of this saponin complex has been recently proposed, in which the β-escin mixture is perceived as a source of a hitherto unavailable raw material, pentacyclic triterpene aglycone-protoescigenin. Although many liquid chromatography methods are described in the literature for saponins determination, analysis of protoescigenin is barely mentioned. In this work, a new ultra-high performance liquid chromatography (UHPLC) method developed for protoescigenin quantification has been described. CAD (charged aerosol detection), as a relatively new detection method based on aerosol charging, has been applied in this method as an alternative to ultraviolet (UV) detection. The influence of individual parameters on CAD response and sensitivity was studied. The detection was performed using CAD and UV (200 nm) simultaneously and the results were compared with reference to linearity, accuracy, precision and limit of detection.
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Repeatability Assessment by ISO 11843-7 in Quantitative HPLC for Herbal Medicines.
Chen, Liangmian; Kotani, Akira; Hakamata, Hideki; Tsutsumi, Risa; Hayashi, Yuzuru; Wang, Zhimin; Kusu, Fumiyo
2015-01-01
We have proposed an assessment methods to estimate the measurement relative standard deviation (RSD) of chromatographic peaks in quantitative HPLC for herbal medicines by the methodology of ISO 11843 Part 7 (ISO 11843-7:2012), which provides detection limits stochastically. In quantitative HPLC with UV detection (HPLC-UV) of Scutellaria Radix for the determination of baicalin, the measurement RSD of baicalin by ISO 11843-7:2012 stochastically was within a 95% confidence interval of the statistically obtained RSD by repetitive measurements (n = 6). Thus, our findings show that it is applicable for estimating of the repeatability of HPLC-UV for determining baicalin without repeated measurements. In addition, the allowable limit of the "System repeatability" in "Liquid Chromatography" regulated in a pharmacopoeia can be obtained by the present assessment method. Moreover, the present assessment method was also successfully applied to estimate the measurement RSDs of quantitative three-channel liquid chromatography with electrochemical detection (LC-3ECD) of Chrysanthemi Flos for determining caffeoylquinic acids and flavonoids. By the present repeatability assessment method, reliable measurement RSD was obtained stochastically, and the experimental time was remarkably reduced.
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Rapid and label-free bioanalytical method of alpha fetoprotein detection using LSPR chip
NASA Astrophysics Data System (ADS)
Kim, Dongjoo; Kim, Jinwoon; Kwak, Cheol Hwan; Heo, Nam Su; Oh, Seo Yeong; Lee, Hoomin; Lee, Go-Woon; Vilian, A. T. Ezhil; Han, Young-Kyu; Kim, Woo-Sik; Kim, Gi-bum; Kwon, Soonjo; Huh, Yun Suk
2017-07-01
Alpha fetoprotein (AFP) is a cancer marker, particularly for hepatocellular carcinoma. Normal levels of AFP are less than 20 ng/mL; however, its levels can reach more than 400 ng/mL in patients with HCC. Enzyme linked immunosorbent assay (ELISA) and radioimmunoassay (RIA) have been employed for clinical diagnosis of AFP; however, these methods are time consuming and labor intensive. In this study, we developed a localized surface plasmon resonance (LSPR) based biosensor for simple and rapid detection of AFP. This biosensor consists of a UV-Vis spectrometer, a cuvette cell, and a biosensor chip nanopatterned with gold nanoparticles (AuNPs). In our LSPR biosensor, binding of AFP to the surface of the sensor chip led to an increasing magnitude of the LSPR signals, which was measured by an ultraviolet-visible (UV-Vis) spectrometer. Our LSPR biosensor showed sufficient detectability of AFP at concentrations of 1 ng/mL to 1 μg/mL. Moreover, the overall procedure for detection of AFP was completed within 20 min. This biosensor could also be utilized for a point of care test (POCT) by employing a portable UV-Vis spectrometer. Owing to the simplicity and rapidity of the detection process, our LSPR biosensor is expected to replace traditional diagnostic methods for the early detection of diseases.
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Zanolari, Boris; Ndjoko, Karine; Ioset, Jean-Robert; Marston, Andrew; Hostettmann, Kurt
2003-01-01
The development and validation of a rapid qualitative and quantitative method based on an HPLC-UV-MS technique with atmospheric pressure chemical ionisation and electrospray ionisation for the analysis of yohimbine in a number of commercial aphrodisiac products is reported. HPLC with multiple-stage mass spectrometry experiments allowed the identification of the target compound and increased the selectivity of complex analyses such as those involved with multi-botanical preparations. The precision and the robustness of the method were improved by the use of two internal standards: codeine for UV detection and deuterium-labelled yohimbine for MS detection. Twenty commercial aphrodisiac preparations were analysed and the amount of yohimbine measured and expressed as the maximal dose per day suggested on product labels ranged from 1.32 to 23.16 mg.
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2014-01-01
Background Trichloroethene and tetrachloroethene are the most common pollutants in groundwater and two of the priority pollutants listed by the U.S. Environmental Protection Agency. In previous studies on TCE and PCE photolysis and photochemical degradation, concentration ranges exceeding environmental levels by far with millimolar concentrations of TCE and PCE have been used, and it is not clear if the obtained results can be used to explain the degradation of these contaminants at more realistic environmental concentration levels. Methods Experiments with micromolar concentrations of TCE and PCE in aqueous solution using direct photolysis and UV/H2O2 have been conducted and product formation as well as transformation efficiency have been investigated. SPME/GC/MS, HPLC/UV and ion chromatography with conductivity detection have been used to determine intermediates of degradation. Results The results showed that chloride was a major end product in both TCE and PCE photodegradation. Several intermediates such as formic acid, dichloroacetic acid, dichloroacetaldehyede, chloroform, formaldehyde and glyoxylic acid were formed during both, UV and UV/H2O2 treatment of TCE. However chloroacetaldehyde and chloroacetic acid were only detected during direct UV photolysis of TCE and oxalic acid was only formed during the UV/H2O2 process. For PCE photodegradation, formic acid, di- and trichloroacetic acids were detected in both UV and UV/H2O2 systems, but formaldehyde and glyoxylic acid were only detected during direct UV photolysis. Conclusions For water treatment UV/H2O2 seems to be favorable over direct UV photolysis because of its higher degradation efficiency and lower risk for the formation of harmful intermediates. PMID:24401763
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Correlation fluorescence method of amine detection
NASA Astrophysics Data System (ADS)
Myslitsky, Valentin F.; Tkachuk, Svetlana S.; Rudeichuk, Volodimir M.; Strinadko, Miroslav T.; Slyotov, Mikhail M.; Strinadko, Marina M.
1997-12-01
The amines fluorescence spectra stimulated by UV laser radiation are investigated in this paper. The fluorescence is stimulated by the coherent laser beam with the wavelength 0.337 micrometers . At the sufficient energy of laser stimulation the narrow peaks of the fluorescence spectra are detected besides the wide maximum. The relationship between the fluorescence intensity and the concentration of amines solutions are investigated. The fluorescence intensity temporal dependence on wavelength 0.363 micrometers of the norepinephrine solution preliminarily radiated by UV laser with wavelength 0.337 micrometers was found. The computer stimulated and experimental investigations of adrenaline and norepinephrine mixtures fluorescence spectra were done. The correlation fluorescent method of amines detection is proposed.
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Mercury speciation by differential photochemical vapor generation at UV-B vs. UV-C wavelength
NASA Astrophysics Data System (ADS)
Chen, Guoying; Lai, Bunhong; Mei, Ni; Liu, Jixin; Mao, Xuefei
2017-11-01
Photochemical vapor generation (PVG) is an effective sample introduction scheme for volatile mercury (Hg). Speciation of Hg++ and MeHg+ was fulfilled for the first time by differential PVG under UV-B vs. UV-C wavelength and applied to fish oil supplements. After liquid-liquid extraction, the aqueous extract was mixed with 0.4% anthranilic acid (AA)-20% formic acid (FA) in a quartz coil, and exposed sequentially to 311 nm or 254 nm UV light. The resulting Hg0 vapor was detected by atomic fluorescence spectrometry (AFS). At each wavelength, the AFS intensity was a linear function of Hg++ and MeHg+ concentrations, which were solvable from a set of two equations. This method achieved ultrahigh sensitivity with 0.50 and 0.63 ng mL- 1 limits of detection for Hg++ and MeHg+, respectively, and 73% recovery for MeHg+ at 10 ng mL- 1. Validation was performed by ICP-MS on total Hg. Obviation of chemical or chromatographic separation rendered this method rapid, green, and cost-effective.
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Ribeiro, T; Depres, S; Couteau, G; Pauss, A
2003-01-01
An alternative method for the estimation of nitrate and nitrogen forms in vegetables is proposed. Nitrate can be directly estimated by UV-spectrophotometry after an extraction step with water. The other nitrogen compounds are photo-oxidized into nitrate, and then estimated by UV-spectrophotometry. An oxidative solution of sodium persulfate and a Hg-UV lamp is used. Preliminary assays were realized with vegetables like salade, spinachs, artichokes, small peas, broccolis, carrots, watercress; acceptable correlations between expected and experimental values of nitrate amounts were obtained, while the detection limit needs to be lowered. The optimization of the method is underway.
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Hess, S; Teubert, U; Ortwein, J; Eger, K
2001-12-01
The anti-inflammatory drug indomethacin was investigated regarding new related impurities. Therefore, related substances 2-9 were prepared by independent synthesis and physicochemically characterized. To determine indomethacin and its related substances, a new HPLC-UV method was developed and validated. Indomethacin and its impurities were eluted on a C(18) column with a mobile phase consisting of methanol and an aqueous solution of 0.2% phosphoric acid at a flow rate of 1.5 ml/min and were quantified by UV detection at 320 nm. Overall, the HPLC-UV method was simple and reliable for the detection of eight impurities in indomethacin. In addition to the HPLC-UV method, 1H nuclear magnetic resonance (NMR) was used to investigate indomethacin regarding impurities. For that purpose, related substances 2-9 were systematically added to indomethacin and investigated. The NMR method was found to be very useful for the identification of impurities in bulk substance without prior separation. Both HPLC-UV and NMR were used to analyze 38 batches of indomethacin available on the European market. The outcome was that 42% of the batches did not meet the compendial requirements although they met the specifications of current compendial methods. Some batches contained the previously undescribed impurity 8, while other batches contained by-products from two distinct synthetic routes. The methods presented herein are important contributions to the ongoing efforts to reduce impurities and therefore the risk of adverse side-effects in drugs that are no longer under patent protection.
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Ferey, Justine; Da Silva, David; Bravo-Veyrat, Sophie; Lafite, Pierre; Daniellou, Richard; Maunit, Benoît
2016-12-16
This paper presents a kinetic study of invertase, a specific fructofuranosidase cloned from the Leishmania major genome. The kinetic parameters of the β-d-fructofuranosidase from Leishmania major (BfrA) were determined using Thin-Layer Chromatography (TLC) and UV-densitometry (TLC@UV) specifically developed for the separation and detection of three carbohydrates namely sucrose, glucose and fructose. Separation was performed on TLC silica gel 60 F254 plates impregnated with sodium bisulphate and citrate and heated prior to development. This fast and easy separation was performed with two successive developments using ACN/H 2 O 80/20 (v/v) as mobile phase. Sensitive and repeatable derivatization of sugars was achieved by dipping the plates in a solution of 4-aminobenzoic acid. Quantification was performed by UV-detection. The method was validated according to ICH guidelines Q2(R1) in terms of specificity, limits of detection and quantification, precision and robustness (with n=3 replicates and CV ≤10%). The characterization of BfrA reaction kinetic was performed by monitoring the accumulation of either glucose or fructose detected by TLC@UV. Hydrolysis of sucrose was described by the Michaelis-Menten kinetic parameters (K M ; V max ) respectively equal to 63.09±7.590mM; 0.037±0.00094mM/min using glucose production and 83.01±14.39mM; 0.031±0.0021mM/min monitoring fructose. Hydrolyses of three alternative substrates, raffinose, stachyose and inulin, were also compared and the regiospecificity of the reaction was characterized. This TLC@UV method is shown to be suitable for the refined kinetic analysis of different reactions related to the hydrolysis of sugars. Copyright © 2016. Published by Elsevier B.V.
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NASA Astrophysics Data System (ADS)
Hadad, Ghada M.; El-Gindy, Alaa; Mahmoud, Waleed M. M.
2008-08-01
High-performance liquid chromatography (HPLC) and multivariate spectrophotometric methods are described for the simultaneous determination of ambroxol hydrochloride (AM) and doxycycline (DX) in combined pharmaceutical capsules. The chromatographic separation was achieved on reversed-phase C 18 analytical column with a mobile phase consisting of a mixture of 20 mM potassium dihydrogen phosphate, pH 6-acetonitrile in ratio of (1:1, v/v) and UV detection at 245 nm. Also, the resolution has been accomplished by using numerical spectrophotometric methods as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS-1) applied to the UV spectra of the mixture and graphical spectrophotometric method as first derivative of the ratio spectra ( 1DD) method. Analytical figures of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of quantitation and limit of detection were determined for CLS, PLS-1 and PCR methods. The proposed methods were validated and successfully applied for the analysis of pharmaceutical formulation and laboratory-prepared mixtures containing the two component combination.
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Hadad, Ghada M; El-Gindy, Alaa; Mahmoud, Waleed M M
2008-08-01
High-performance liquid chromatography (HPLC) and multivariate spectrophotometric methods are described for the simultaneous determination of ambroxol hydrochloride (AM) and doxycycline (DX) in combined pharmaceutical capsules. The chromatographic separation was achieved on reversed-phase C(18) analytical column with a mobile phase consisting of a mixture of 20mM potassium dihydrogen phosphate, pH 6-acetonitrile in ratio of (1:1, v/v) and UV detection at 245 nm. Also, the resolution has been accomplished by using numerical spectrophotometric methods as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS-1) applied to the UV spectra of the mixture and graphical spectrophotometric method as first derivative of the ratio spectra ((1)DD) method. Analytical figures of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of quantitation and limit of detection were determined for CLS, PLS-1 and PCR methods. The proposed methods were validated and successfully applied for the analysis of pharmaceutical formulation and laboratory-prepared mixtures containing the two component combination.
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Moncrieff, J
1994-03-18
A simple, extractionless method for the determination of dapsone in serum and saliva is described. Reversed-phase high-performance liquid chromatography is used with UV detection at 295 nm or electrochemical detection at 0.7 V. Diazoxide in buffer is the internal standard for UV detection and practolol for electrochemical detection. Sample preparation is minimal with protein precipitation of serum samples whilst saliva samples are simply diluted with addition of an internal standard. Low-level serum and saliva samples are front-cut on-line with a 3 cm laboratory-made precolumn in the loop position on a standard Valco injection valve. Isocratic separation is achieved on a 250 mm x 4.6 mm I.D. stainless-steel Spherisorb S5 ODS-1 column. The mobile phase for high levels of dapsone is acetonitrile-elution buffer (12:88, v/v) at 2 ml/min and a column temperature of 40 degrees C for both serum and saliva separations. For the low-level assays using electrochemical detection and solid-phase clean-up, the mobile phase is acetonitrile-methanol-elution buffer (9:4:87, v/v/v). The UV and electrochemical detection limits are 25 ng/ml and 200 pg/ml, respectively, in both serum and saliva. This simple method is applicable to the routine monitoring of dapsone levels in serum from leprotic patients and electrochemical detection gives a simple, reliable method for the monitoring of trough values in subjects on anti-malarial prophylaxis.
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NASA Astrophysics Data System (ADS)
Deng, Chaoxu; Shao, Bingyao; Zhao, Dan; Zhou, Dianli; Yu, Junsheng
2017-11-01
Organic optoelectronic integrated device (OID) with both ultraviolet (UV) detective and electroluminescent (EL) properties was fabricated by using a thermally activated delayed fluorescence (TADF) semiconductor of (4s, 6s)-2,4,5,6-tetra(9H-carbazol-9-yl)isophthalonitrile (4CzIPN) as an emitter. The effect of five kinds of n-type organic semiconductors (OSCs) on the enhancement of UV detective and EL properties of OID was systematically studied. The result shows that two orders of magnitude in UV detectivity from 109 to 1011 Jones and 3.3 folds of luminance from 2499 to 8233 cd m-2 could be achieved. The result shows that not only the difference of lowest unoccupied molecular orbital (LUMO) between active layer and OSC but also the variety of electron mobility have a significant effect on the UV detective and EL performance through adjusting electron injection/transport. Additionally, the optimized OSC thickness is beneficial to confine the leaking of holes from the active layer to cathode, leading to the decrease of dark current for high detective performance. This work provides a useful method on broadening OSC material selection and device architecture construction for the realization of high performance OID.
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Herzog, Bastian; Lemmer, Hilde; Horn, Harald; Müller, Elisabeth
2014-02-22
Evaluation of xenobiotics biodegradation potential, shown here for benzotriazoles (corrosion inhibitors) and sulfamethoxazole (sulfonamide antibiotic) by microbial communities and/or pure cultures normally requires time intensive and money consuming LC/GC methods that are, in case of laboratory setups, not always needed. The usage of high concentrations to apply a high selective pressure on the microbial communities/pure cultures in laboratory setups, a simple UV-absorbance measurement (UV-AM) was developed and validated for screening a large number of setups, requiring almost no preparation and significantly less time and money compared to LC/GC methods. This rapid and easy to use method was evaluated by comparing its measured values to LC-UV and GC-MS/MS results. Furthermore, its application for monitoring and screening unknown activated sludge communities (ASC) and mixed pure cultures has been tested and approved to detect biodegradation of benzotriazole (BTri), 4- and 5-tolyltriazole (4-TTri, 5-TTri) as well as SMX. In laboratory setups, xenobiotics concentrations above 1.0 mg L(-1) without any enrichment or preparation could be detected after optimization of the method. As UV-AM does not require much preparatory work and can be conducted in 96 or even 384 well plate formats, the number of possible parallel setups and screening efficiency was significantly increased while analytic and laboratory costs were reduced to a minimum.
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2014-01-01
Background Evaluation of xenobiotics biodegradation potential, shown here for benzotriazoles (corrosion inhibitors) and sulfamethoxazole (sulfonamide antibiotic) by microbial communities and/or pure cultures normally requires time intensive and money consuming LC/GC methods that are, in case of laboratory setups, not always needed. Results The usage of high concentrations to apply a high selective pressure on the microbial communities/pure cultures in laboratory setups, a simple UV-absorbance measurement (UV-AM) was developed and validated for screening a large number of setups, requiring almost no preparation and significantly less time and money compared to LC/GC methods. This rapid and easy to use method was evaluated by comparing its measured values to LC-UV and GC-MS/MS results. Furthermore, its application for monitoring and screening unknown activated sludge communities (ASC) and mixed pure cultures has been tested and approved to detect biodegradation of benzotriazole (BTri), 4- and 5-tolyltriazole (4-TTri, 5-TTri) as well as SMX. Conclusions In laboratory setups, xenobiotics concentrations above 1.0 mg L-1 without any enrichment or preparation could be detected after optimization of the method. As UV-AM does not require much preparatory work and can be conducted in 96 or even 384 well plate formats, the number of possible parallel setups and screening efficiency was significantly increased while analytic and laboratory costs were reduced to a minimum. PMID:24558966
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Ding, Xuelu; Gerbig, Stefanie; Spengler, Bernhard; Schulz, Sabine
2018-02-01
Organic UV filters in personal care products (PCPs) have been persistently reported as a potential threat to human health. In order to guarantee consumers ' safety, the dose of these compounds in PCPs needs to be monitored. Here, a methodology based on reactive low temperature plasma ionization (LTP) mass spectrometry (MS) has been developed for the determination of common organic UV filters in PCPs including benzophenone-3, ethylhexyl dimethyl p-aminobenzoic acid, ethylhexyl methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, and ethylhexyl salicylate. The experiments were carried out in transmission geometry where the LTP ion source, samples loaded on a stainless steel mesh, and the MS inlet were aligned coaxially. Four chemicals, ammonia, ammonium formate, aniline, and methylamine were considered as reactive additives allowing reactions with the UV filters through different mechanisms. Methylamine-induced reactive LTP-MS showed the most prominent improvement on the detection of UV filter compounds. Compared to direct LTP-MS, the developed method improved the detection limits of UV filters more than 10 fold. Moreover, the method enabled fast semi-quantitative screening of UV filters in authentic PCPs. Concentrations of active ingredients in eight authentic PCPs as determined with reactive LTP-MS were found comparable to values offered by the cosmetic companies and corresponding HPLC data. The methodology provides high throughput analysis (70s per sample) and sensitive identification of organic UV filters. Lowest detectable concentrations ranged from 0.13µg/g for 4-methylbenzylidene camphor to 7.67µg/g for octocrylene in spiked cream. In addition, it shows the potential to be used as a screening tool for legal authentications of these chemicals in the future due to its semi-quantitative determination of UV filters in PCPs without tedious sample preparation and time-consuming chromatographic separation. Copyright © 2017 Elsevier B.V. All rights reserved.
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Kim, Dojung; Kim, Sangseop; Kim, Seol-A; Choi, Myoengsin; Kwon, Kyoung-Jin; Kim, Mijeong; Kim, Dong-Sup; Kim, Seung-Hee; Choi, Bo-Kyung
2012-01-01
Sixteen UV filters were simultaneously analyzed using the high-performance liquid chromatographic method. They were drometrizole (USAN Drometrizole), 4-methylbenzylidene camphor (USAN Enzacamene), menthyl anthranilate (USAN Menthyl anthranilate), benzophenone-3 (USAN Oxybenzone), benzophenone-8 (USAN Dioxybenzone), butyl methoxydibenzoylmethane (USAN Avobenzone), ethylhexyl triazone (USAN Octyl triazone), octocrylene (USAN Octocrylene), ethylhexyl dimethyl p-aminobenzoic acid (USAN Padimate O), ethylhexyl methoxycinnamate (USAN Octinoxate), p-aminobenzoic acid (USAN Aminobenzoic acid), 2-phenylbenzimidazole-5-sulfonic acid (USAN Ensulizole), isoamyl p-methoxycinnamate (USAN Amiloxate), and recent UV filters such as diethylhexyl butamidotriazone (USAN Iscotrizinol), methylene bis-benzotriazolyl tetramethylbutylphenol (USAN Bisoctrizole), and terephthalylidene dicamphor sulfonic acid (USAN Ecamsule). Separation of the UV filters was carried out in a C(18) column with a gradient of methanol-phosphate buffer, and the UV detection was at 300, 320, or 360 nm without any interference. The limits of detection were between 0.08 and 1.94 μg/ml, and the limits of quantitation were between 0.24 and 5.89 μg/ml. The extracting solvent for the UV filters was methanol, except for ethylhexyl triazone and methylene bis-benzotriazolyl tetramethylbutylphenol, which were prepared with tetrahydrofuran. The recoveries from spiked samples were between 94.90% and 116.54%, depending on the matrixes used. The developed method was applied to 23 sunscreens obtained from local markets, and the results were acceptable to their own criteria and to maximum authorized concentrations. Consequently, these results would provide a simple extracting method and a simultaneous determination for various UV filters, which can improve the quality control process as well as the environmental monitoring of sunscreens.
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Comparison of detection techniques for capillary electrophoresis analysis of gold nanoparticles.
Matczuk, Magdalena; Aleksenko, Svetlana S; Matysik, Frank-Michael; Jarosz, Maciej; Timerbaev, Andrei R
2015-05-01
As metallic nanoparticles are growing in importance as analytes in CE, increases an interest in appropriate detection methods for their quantification in various samples. For gold nanoparticles (AuNPs), the most common UV detection poses intricacy of inadequate sensitivity that hinders the applicability of CE. With the objective of resolving this challenge, UV detection was compared with C(4) D and ICP-MS as alternative modes of detection for AuNPs. A C(4) D detector, applied under pressure-driven conditions, exhibited better sensitivity than a UV detector. However, C(4) D turned to be unsatisfactory to differentiate the signal of AuNPs at common CE conditions despite varying the nature of BGE and detection conditions. Due to intrinsic sensitivity and low background levels typical to Au, ICP-MS greatly surpasses UV detection. After optimization trials, CE-ICP-MS gained the LOD of AuNPs as low as 2 × 10(-15) M, as well as an excellent performance in terms of signal stability and linearity. Also importantly, the optimized BGE appears to be well matched to explore the behavior of AuNPs in biologically relevant systems. This was demonstrated by probing the interaction between AuNPs and the main blood-transporting protein, HSA. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Recent developments in optical detection methods for microchip separations.
Götz, Sebastian; Karst, Uwe
2007-01-01
This paper summarizes the features and performances of optical detection systems currently applied in order to monitor separations on microchip devices. Fluorescence detection, which delivers very high sensitivity and selectivity, is still the most widely applied method of detection. Instruments utilizing laser-induced fluorescence (LIF) and lamp-based fluorescence along with recent applications of light-emitting diodes (LED) as excitation sources are also covered in this paper. Since chemiluminescence detection can be achieved using extremely simple devices which no longer require light sources and optical components for focusing and collimation, interesting approaches based on this technique are presented, too. Although UV/vis absorbance is a detection method that is commonly used in standard desktop electrophoresis and liquid chromatography instruments, it has not yet reached the same level of popularity for microchip applications. Current applications of UV/vis absorbance detection to microchip separations and innovative approaches that increase sensitivity are described. This article, which contains 85 references, focuses on developments and applications published within the last three years, points out exciting new approaches, and provides future perspectives on this field.
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da Silva, Claudia Pereira; Emídio, Elissandro Soares; de Marchi, Mary Rosa Rodrigues
2015-01-01
This paper describes the validation of a method consisting of solid-phase extraction followed by gas chromatography-tandem mass spectrometry for the analysis of the ultraviolet (UV) filters benzophenone-3, ethylhexyl salicylate, ethylhexyl methoxycinnamate and octocrylene. The method validation criteria included evaluation of selectivity, analytical curve, trueness, precision, limits of detection and limits of quantification. The non-weighted linear regression model has traditionally been used for calibration, but it is not necessarily the optimal model in all cases. Because the assumption of homoscedasticity was not met for the analytical data in this work, a weighted least squares linear regression was used for the calibration method. The evaluated analytical parameters were satisfactory for the analytes and showed recoveries at four fortification levels between 62% and 107%, with relative standard deviations less than 14%. The detection limits ranged from 7.6 to 24.1 ng L(-1). The proposed method was used to determine the amount of UV filters in water samples from water treatment plants in Araraquara and Jau in São Paulo, Brazil. Copyright © 2014 Elsevier B.V. All rights reserved.
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Kamal, Atif; Gulfraz, Mohammad; Anwar, Mohammad Asad; Malik, Riffat Naseem
2015-01-01
1-hydroxypyrene is an important biomarker of exposure to polycyclic aromatic hydrocarbons (PAHs), which appears in the urine of exposed human subjects. In developing countries, where advanced instruments are not available, the importance of this biomarker demands convenient and sensitive methods for determination purposes. This study aimed at developing a methodology to quantify 1-hydroxypyrene (a biomarker of PAHs exposure) based on the UV-visible detector in the reverse phase high pressure liquid chromatography (HPLC). A 20 μl injection of sample was used for manual injection into the HPLC Shimadzu, equipped with the SPD-20 A UV-visible detector, the LC-20AT pump and the DGU-20A5 degasser. The C-18 column was used for the purpose of the analysis. The method showed a good linearity (the range: R2 = 0.979-0.989), and high detectability up to the nmol level. The average retention was 6.37, with the accuracy of 2%, and the percentage of recovery remained 108%. The overall performance of this method was comparable (in terms of detection sensitivity) and relatively better than previously reported studies using the HPLC system equipped with the UV-detector. This method is suitable and reliable for the detection/quantification of the 1-OHP in human urine samples, using the UV-detector, however, it is less sensitive as compared to the results of a florescence detector. This work is available in Open Access model and licensed under a CC BY-NC 3.0 PL license.
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Carvalho, Melina G.; Aragão, Cícero F. S; Raffin, Fernanda N.; de L. Moura, Túlio F. A.
2017-01-01
Topical gels containing extracts of Schinus terebinthifolius have been used to treat bacterial vaginosis. It has been reported that this species has antimicrobial, anti-inflammatory and anti-ulcerogenic properties, which can be attributed to the presence of phenolic compounds. In this work, a sensitive and selective reversed-phase HPLC-UV/DAD method for the simultaneous assay of six polyphenols that could be present in S. terebinthifolius was developed. The method was shown to be accurate and precise. Peak purity and similarity index both exceeded 0.99. Calibration curves were linear over the concentration range studied, with correlation coefficients between 0.9931 and 0.9974. This method was used to determine the polyphenol content of a hydroalcoholic extract and pharmacy-compounded vaginal gel. Although the method is useful to assess the 6 phenolic compounds, some compounds could not be detected in the products. SUMMARY A sensitive, selective, accurate and precise reversed-phase HPLC-UV/DAD method for the simultaneous assay of six polyphenols in S. terebinthifolius Raddi Abbreviations used: RP-HPLC-UV/DAD: Reverse Phase High Performance Liquid Chromatograph with Ultraviolet and Diode Array Detector, HPLC: High Performance Liquid Chromatograph, HPLC-UV: High Performance Liquid Chromatograph with Ultraviolet Detector, ANVISA: Brazilian National Health Surveillance Agency, LOD: Limit of detection, LOQ: Limit of quantitation PMID:28539726
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Tang, Bin; Wei, Biao; Wu, De-Cao; Mi, De-Ling; Zhao, Jing-Xiao; Feng, Peng; Jiang, Shang-Hai; Mao, Ben-Jiang
2014-11-01
Eliminating turbidity is a direct effect spectroscopy detection of COD key technical problems. This stems from the UV-visible spectroscopy detected key quality parameters depend on an accurate and effective analysis of water quality parameters analytical model, and turbidity is an important parameter that affects the modeling. In this paper, we selected formazine turbidity solution and standard solution of potassium hydrogen phthalate to study the turbidity affect of UV--visible absorption spectroscopy detection of COD, at the characteristics wavelength of 245, 300, 360 and 560 nm wavelength point several characteristics with the turbidity change in absorbance method of least squares curve fitting, thus analyzes the variation of absorbance with turbidity. The results show, In the ultraviolet range of 240 to 380 nm, as the turbidity caused by particle produces compounds to the organics, it is relatively complicated to test the turbidity affections on the water Ultraviolet spectra; in the visible region of 380 to 780 nm, the turbidity of the spectrum weakens with wavelength increases. Based on this, this paper we study the multiplicative scatter correction method affected by the turbidity of the water sample spectra calibration test, this method can correct water samples spectral affected by turbidity. After treatment, by comparing the spectra before, the results showed that the turbidity caused by wavelength baseline shift points have been effectively corrected, and features in the ultraviolet region has not diminished. Then we make multiplicative scatter correction for the three selected UV liquid-visible absorption spectroscopy, experimental results shows that on the premise of saving the characteristic of the Ultraviolet-Visible absorption spectrum of water samples, which not only improve the quality of COD spectroscopy detection SNR, but also for providing an efficient data conditioning regimen for establishing an accurate of the chemical measurement methods.
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NASA Astrophysics Data System (ADS)
Ganot, Noam; Gal-Yam, Avishay; Ofek, Eran. O.; Sagiv, Ilan; Waxman, Eli; Lapid, Ofer; Kulkarni, Shrinivas R.; Ben-Ami, Sagi; Kasliwal, Mansi M.; The ULTRASAT Science Team; Chelouche, Doron; Rafter, Stephen; Behar, Ehud; Laor, Ari; Poznanski, Dovi; Nakar, Ehud; Maoz, Dan; Trakhtenbrot, Benny; WTTH Consortium, The; Neill, James D.; Barlow, Thomas A.; Martin, Christofer D.; Gezari, Suvi; the GALEX Science Team; Arcavi, Iair; Bloom, Joshua S.; Nugent, Peter E.; Sullivan, Mark; Palomar Transient Factory, The
2016-03-01
The radius and surface composition of an exploding massive star, as well as the explosion energy per unit mass, can be measured using early UV observations of core-collapse supernovae (SNe). We present the first results from a simultaneous GALEX/PTF search for early ultraviolet (UV) emission from SNe. Six SNe II and one Type II superluminous SN (SLSN-II) are clearly detected in the GALEX near-UV (NUV) data. We compare our detection rate with theoretical estimates based on early, shock-cooling UV light curves calculated from models that fit existing Swift and GALEX observations well, combined with volumetric SN rates. We find that our observations are in good agreement with calculated rates assuming that red supergiants (RSGs) explode with fiducial radii of 500 R ⊙, explosion energies of 1051 erg, and ejecta masses of 10 M ⊙. Exploding blue supergiants and Wolf-Rayet stars are poorly constrained. We describe how such observations can be used to derive the progenitor radius, surface composition, and explosion energy per unit mass of such SN events, and we demonstrate why UV observations are critical for such measurements. We use the fiducial RSG parameters to estimate the detection rate of SNe during the shock-cooling phase (<1 day after explosion) for several ground-based surveys (PTF, ZTF, and LSST). We show that the proposed wide-field UV explorer ULTRASAT mission is expected to find >85 SNe per year (˜0.5 SN per deg2), independent of host galaxy extinction, down to an NUV detection limit of 21.5 mag AB. Our pilot GALEX/PTF project thus convincingly demonstrates that a dedicated, systematic SN survey at the NUV band is a compelling method to study how massive stars end their life.
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Khokhra, Richa; Bharti, Bandna; Lee, Heung-No; Kumar, Rajesh
2017-11-08
This study demonstrates significant visible light photo-detection capability of pristine ZnO nanostructure thin films possessing substantially high percentage of oxygen vacancies [Formula: see text] and zinc interstitials [Formula: see text], introduced by simple tuning of economical solution method. The demonstrated visible light photo-detection capability, in addition to the inherent UV light detection ability of ZnO, shows great dependency of [Formula: see text] and [Formula: see text] with the nanostructure morphology. The dependency was evaluated by analyzing the presence/percentage of [Formula: see text] and [Formula: see text] using photoluminescence (PL) and X-ray photoelectron spectroscopy (XPS) measurements. Morphologies of ZnO viz. nanoparticles (NPs), nanosheets (NSs) and nanoflowers (NFs), as a result of tuning of synthesis method contended different concentrations of defects, demonstrated different photo-detection capabilities in the form of a thin film photodetector. The photo-detection capability was investigated under different light excitations (UV; 380~420 nm, white ; λ > 420 nm and green; 490~570 nm). The as fabricated NSs photodetector possessing comparatively intermediate percentage of [Formula: see text] ~ 47.7% and [Formula: see text] ~ 13.8% exhibited superior performance than that of NPs and NFs photodetectors, and ever reported photodetectors fabricated by using pristine ZnO nanostructures in thin film architecture. The adopted low cost and simplest approach makes the pristine ZnO-NSs applicable for wide-wavelength applications in optoelectronic devices.
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Li, Yi; Zhang, Min; Yang, Yaoxia; Wang, Xuemei; Du, Xinzhen
2014-09-05
A novel TiO2-nanosheets coated fiber for solid-phase microextraction (SPME) was fabricated by anodization of Ti wire substrates in ethylene glycol with concentrated NH4F. The in situ fabricated TiO2-nanosheets were densely embedded into Ti substrates with about 1μm long, 300nm wide and 80nm thick. The as-fabricated TiO2-nanosheets coating was employed to extract polycyclic aromatic hydrocarbons, phthalates and ultraviolet (UV) filters in combination with high performance liquid chromatography-UV detection (HPLC-UV). It was found that the TiO2-nanosheets coating exhibited high extraction capability and good selectivity for some UV filters frequently used in cosmetic sunscreen formulations. The main parameters affecting extraction performance were investigated and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.1-400μgL(-1). The limits of detection of the proposed method were between 0.026μgL(-1) and 0.089μgL(-1) (S/N=3). The single fiber repeatability varied from 4.50% to 8.76% and the fiber-to-fiber reproducibility ranged from 7.75% to 9.64% for the extraction of spiked water with 50μgL(-1) UV filters (n=5). The SPME-HPLC-UV method was successfully established for the selective preconcentration and sensitive detection of target UV filters from real environmental water samples. Recovery of UV filters spiked at 10μgL(-1) and 25μgL(-1) ranged from 88.8% to 107% and the relative standard deviations were less than 9.8%. Furthermore the in situ growth of the TiO2-nanosheets coating was performed in a highly reproducible manner and the TiO2-nanosheets coated fiber has high mechanical strength, good stability and long service life. Copyright © 2014 Elsevier B.V. All rights reserved.
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The Classification of Ground Roasted Decaffeinated Coffee Using UV-VIS Spectroscopy and SIMCA Method
NASA Astrophysics Data System (ADS)
Yulia, M.; Asnaning, A. R.; Suhandy, D.
2018-05-01
In this work, an investigation on the classification between decaffeinated and non- decaffeinated coffee samples using UV-VIS spectroscopy and SIMCA method was investigated. Total 200 samples of ground roasted coffee were used (100 samples for decaffeinated coffee and 100 samples for non-decaffeinated coffee). After extraction and dilution, the spectra of coffee samples solution were acquired using a UV-VIS spectrometer (Genesys™ 10S UV-VIS, Thermo Scientific, USA) in the range of 190-1100 nm. The multivariate analyses of the spectra were performed using principal component analysis (PCA) and soft independent modeling of class analogy (SIMCA). The SIMCA model showed that the classification between decaffeinated and non-decaffeinated coffee samples was detected with 100% sensitivity and specificity.
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Cao, Mingyan; Mo, Wenjun David; Shannon, Anthony; Wei, Ziping; Washabaugh, Michael; Cash, Patricia
Aspartate (Asp) isomerization is a common post-translational modification of recombinant therapeutic proteins that can occur during manufacturing, storage, or administration. Asp isomerization in the complementarity-determining regions of a monoclonal antibody may affect the target binding and thus a sufficiently robust quality control method for routine monitoring is desirable. In this work, we utilized a liquid chromatography-mass spectrometry (LC/MS)-based approach to identify the Asp isomerization in the complementarity-determining regions of a therapeutic monoclonal antibody. To quantitate the site-specific Asp isomerization of the monoclonal antibody, a UV detection-based quantitation assay utilizing the same LC platform was developed. The assay was qualified and implemented for routine monitoring of this product-specific modification. Compared with existing methods, this analytical paradigm is applicable to identify Asp isomerization (or other modifications) and subsequently develop a rapid, sufficiently robust quality control method for routine site-specific monitoring and quantitation to ensure product quality. This approach first identifies and locates a product-related impurity (a critical quality attribute) caused by isomerization, deamidation, oxidation, or other post-translational modifications, and then utilizes synthetic peptides and MS to assist the development of a LC-UV-based chromatographic method that separates and quantifies the product-related impurities by UV peaks. The established LC-UV method has acceptable peak specificity, precision, linearity, and accuracy; it can be validated and used in a good manufacturing practice environment for lot release and stability testing. Aspartate isomerization is a common post-translational modification of recombinant proteins during manufacture process and storage. Isomerization in the complementarity-determining regions (CDRs) of a monoclonal antibody A (mAb-A) has been detected and has been shown to have impact on the binding affinity to the antigen. In this work, we utilized a mass spectrometry-based peptide mapping approach to detect and quantitate the Asp isomerization in the CDRs of mAb-A. To routinely monitor the CDR isomerization of mAb-A, a focused peptide mapping method utilizing reversed phase chromatographic separation and UV detection has been developed and qualified. This approach is generally applicable to monitor isomerization and other post-translational modifications of proteins in a specific and high-throughput mode to ensure product quality. © PDA, Inc. 2016.
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Gumuslu, Saadet; Yucel, Gultekin; Sarikcioglu, Sureyya Bilmen; Serteser, Mustafa
2005-01-01
A chemiluminescence (CL) technique, which determines the glucose-6-phosphate dehydrogenase (G-6-PD) activities in healthy, heterozygous, and completely enzyme-deficient individuals was applied. CL intensities were detected for 4 h at 15-min intervals in each sample with or without addition of G-6-PD substrates into the reaction mixture. The results revealed an inverse correlation to the reference UV method (Zinkham method; r=-0.80). Furthermore, the CL assay was able to detect G-6-PD activities as low as 0.2 IU/gHb, which was not possible by the UV method. In conclusion, we believe that this method offers a new diagnostic tool for the detection of G-6-PD activities in enzyme-deficient individuals and, because of its increased sensitivity, makes it amenable for determining the effects of different pharmaceutical agents on G-6-PD activity in tissue or cell cultures.
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Joy, Abraham; Anim-Danso, Emmanuel; Kohn, Joachim
2009-01-01
Methods for the detection and estimation of diphosgene and triphosgene are described. These compounds are widely used phosgene precursors which produce an intensely colored purple pentamethine oxonol dye when reacted with 1,3-dimethylbarbituric acid (DBA) and pyridine (or a pyridine derivative). Two quantitative methods are described, based on either UV absorbance or fluorescence of the oxonol dye. Detection limits are ~ 4 µmol/L by UV and <0.4 µmol/L by fluorescence. The third method is a test strip for the simple and rapid detection and semi-quantitative estimation of diphosgene and triphosgene, using a filter paper embedded with dimethylbarbituric acid and poly(4-vinylpyridine). Addition of a test solution to the paper causes a color change from white to light blue at low concentrations and to pink at higher concentrations of triphosgene. The test strip is useful for quick on-site detection of triphosgene and diphosgene in reaction mixtures. The test strip is easy to perform and provides clear signal readouts indicative of the presence of phosgene precursors. The utility of this method was demonstrated by the qualitative determination of residual triphosgene during the production of poly(Bisphenol A carbonate). PMID:19782219
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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.
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De Orsi, Daniela; Pellegrini, Manuela; Pichini, Simona; Mattioli, Donatella; Marchei, Emilia; Gagliardi, Luigi
2008-11-04
A simple high-performance liquid chromatography (HPLC) method with ultraviolet diode array (UV-DAD) and electrospray ionisation mass spectrometry (ESI-MS) detection has been developed for the determination of minoxidil, progesterone, estrone, spironolactone, canrenone, hydrocortisone and triamcinolone acetonide in cosmetic products. The presence of these substances in commercial cosmetic samples is prohibited. The compounds were separated by reversed phase chromatography with water (0.1% trifluoroacetic acid) and acetonitrile gradient elution and detected by UV-DAD at 230, 254 and 280 nm and by ESI-MS positive ionisation mode. Benzoic acid was used as internal standard. Linearity was studied with UV-DAD detection from 1.50 to 1,000 microg/ml or mug/g range, depending on the different compounds and type of cosmetic preparation and with ESI-MS in the 50-1,000 ng/ml or ng/g range. Good determination coefficients (r(2)>or=0.99) were found in both UV and ESI-MS. At three concentrations spanning the linear dynamic ranges of both UV-DAD and ESI-MS assay, mean recoveries were always higher than 90% for the different analytes. This method was successfully applied to the analysis of substances under investigations illegally added in cosmetic cream and lotions, sold on internet web sites to prevent hair loss and other hormone-dependent skin diseases, like acne and hirsutism.
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Colombo, Renata; Lanças, Fernando M; Yariwake, Janete H
2006-01-20
A high-performance liquid chromatography (HPLC) method with photo-diode array (DAD) detection was developed to separate and quantify flavonoids in sugarcane leaves and bagasse (= the crushed sugarcane refuse from juice extraction), and in sugarcane juice. Sugarcane flavonoids consist of a complex mixture of aglycones and glycosides (including flavonolignan glycosides), and the HPLC-UV method herein proposed is suitable for their quantification as total flavonoids. This method was applied to analyze samples of cultivated sugarcane, commercial juice and transgenic sugarcane leaves. Sugarcane leaves proved a promising source of flavonoids: an average of 1.10 mg of total flavonoids/g plant material was found in fresh leaves. Moreover, the flavonoid content of sugarcane juice (0.6 mg/mL) is comparable to other food sources of flavonoids previously reported. Transgenic sugarcane leaves ("Bowman-Birk" and "Kunitz") were compared with non-modified ("control") plant samples using the proposed HPLC-UV method, which indicated that the content of total flavonoids in transgenic plants is different from that in non-modified sugarcane.
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Gonzalez, Oriol; Roso, Sergio; Vilanova, Xavier; Llobet, Eduard
2016-01-01
We report on the use of combined heating and pulsed UV light activation of indium oxide gas sensors for enhancing their performance in the detection of nitrogen dioxide in air. Indium oxide nano-octahedra were synthesized at high temperature (900 °C) via vapour-phase transport and screen-printed onto alumina transducers that comprised interdigitated electrodes and a heating resistor. Compared to the standard, constant temperature operation of the sensor, mild heating (e.g., 100 °C) together with pulsed UV light irradiation employing a commercially available, 325 nm UV diode (square, 1 min period, 15 mA drive current signal), results in an up to 80-fold enhancement in sensitivity to nitrogen dioxide. Furthermore, this combined operation method allows for making savings in power consumption that range from 35% to over 80%. These results are achieved by exploiting the dynamics of sensor response under pulsed UV light, which convey important information for the quantitative analysis of nitrogen dioxide.
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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.
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Bruno, Sergio N F; Cardoso, Carlos R; Maciel, Márcia Mosca A; Vokac, Lidmila; da Silva Junior, Ademário I
2014-09-15
High-pressure liquid chromatography with ultra-violet detection (HPLC-UV) is one of the most commonly used methods to identify and quantify saccharin in non-alcoholic beverages. However, due to the wide variety of interfering UV spectra in saccharin-containing beverage matrices, the same method cannot be used to measure this analyte accurately. We have developed a new, highly effective method to identify and quantify saccharin using HPLC with fluorescence detection (HPLC-FLD). The excitation wavelength (250 nm) and emission wavelength (440 nm) chosen increased selectivity for all matrices and ensured few changes were required in the mobile phase or other parameters. The presence of saccharin in non-diet beverages - a fraud commonly used to replace more expensive sucrose - was confirmed by comparing coincident peaks as well as the emission spectra of standards and samples. Copyright © 2014 Elsevier Ltd. All rights reserved.
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Carmo, Ana Paula Barbosa do; Borborema, Manoella; Ribeiro, Stephan; De-Oliveira, Ana Cecilia Xavier; Paumgartten, Francisco Jose Roma; Moreira, Davyson de Lima
2017-01-01
Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD) and quantification (LOQ) limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral) PQ diphosphate. By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.
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Zamora, D; Torres, A
2014-01-01
Reliable estimations of the evolution of water quality parameters by using in situ technologies make it possible to follow the operation of a wastewater treatment plant (WWTP), as well as improving the understanding and control of the operation, especially in the detection of disturbances. However, ultraviolet (UV)-Vis sensors have to be calibrated by means of a local fingerprint laboratory reference concentration-value data-set. The detection of outliers in these data-sets is therefore important. This paper presents a method for detecting outliers in UV-Vis absorbances coupled to water quality reference laboratory concentrations for samples used for calibration purposes. Application to samples from the influent of the San Fernando WWTP (Medellín, Colombia) is shown. After the removal of outliers, improvements in the predictability of the influent concentrations using absorbance spectra were found.
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Fukushi, Keiichi; Ito, Hideyuki; Kimura, Kenichi; Yokota, Kuriko; Saito, Keiitsu; Chayama, Kenji; Takeda, Sahori; Wakida, Shin-ichi
2006-02-17
We developed capillary zone electrophoresis (CZE) with direct UV detection for determination of ammonium in environmental water samples. Ammonium in the samples was partly converted into ammonia in the alkaline background electrolyte (BGE) during migration and was detected by molecular absorption of ammonia at 190 nm in approximately 7 min. The limit of detection (LOD) for ammonium was 0.24 mg/l (as nitrogen) at a signal-to-noise ratio of three. The respective values of the relative standard deviation (RSD) of peak area, peak height, and migration time for ammonium were 2.1, 1.8, and 0.46%. Major alkali and alkaline earth metal ions coexisting in the samples did not interfere with ammonium determination by the proposed method. The proposed method determined ammonium in surface water and sewage samples. The results were compared to those obtained using ion chromatography (IC).
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Development of high power UV irradiance meter calibration device
NASA Astrophysics Data System (ADS)
Xia, Ming; Gao, Jianqiang; Yin, Dejin; Li, Tiecheng
2016-09-01
With the rapid development of China's economy, many industries have more requirements for UV light applications, such as machinery manufacturing, aircraft manufacturing using high power UV light for detection, IT industry using high power UV light for curing component assembly, building materials, ink, paint and other industries using high power UV light for material aging test etc. In these industries, there are many measuring instruments for high power UV irradiance which are need to traceability. But these instruments are mostly imported instruments, these imported UV radiation meter are large range, wide wavelength range and high accuracy. They have exceeded our existing calibration capability. Expand the measuring range and improve the measurement accuracy of UV irradiance calibration device is a pressing matter of the moment. The newly developed high power UV irradiance calibration device is mainly composed of high power UV light, UV filter, condenser, UV light guide, optical alignment system, standard cavity absolute radiometer. The calibration device is using optical alignment system to form uniform light radiation field. The standard is standard cavity absolute radiometer, which can through the electrical substitution method, by means of adjusting and measuring the applied DC electric power at the receiver on a heating wire, which is equivalent to the thermo-electromotive force generated by the light radiation power, to achieve absolute optical radiation measurement. This method is the commonly used effective method for accurate measurement of light irradiation. The measuring range of calibration device is (0.2 200) mW/cm2, and the uncertainty of measurement results can reached 2.5% (k=2).
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NASA Astrophysics Data System (ADS)
Bacon, Christina P.; Rose, J. B.; Patten, K.; Garcia-Rubio, Luis H.
1995-05-01
Cryptosporidium and Giardia are enteric protozoa which cause waterborne diseases. To date, the detection of these organisms in water has relied upon microscopic immunofluorescent assay technology which uses antibodies directed against the cyst and oocyst forms of the protozoa. In this paper, the uv/vis extinction spectra of aqueous dispersions of Cryptosporidium and Giardia have been studied to investigate the potential use of light scattering-spectral deconvolution techniques as a rapid method for the identification and quantification of protozoa in water. Examination of purified samples of Cryptosporidium and Giardia suggests that spectral features apparent in the short wavelength region of the uv/vis spectra contain information that may be species specific for each protozoa. The spectral characteristics, as well as the particle size analysis, determined from the same spectra, allow for the quantitative classification, identification, and possibly, the assessment of the viability of the protozoa. To further increase the sensitivity of this technique, specific antibodies direction against these organisms, labelled with FITC and rhodamine are being used. It is demonstrated that uv/vis spectroscopy provides an alternative method for the characterization of Giardia and Cryptosporidium. The simplicity and reproducibility of uv/vis spectroscopy measurements makes this technique ideally suited for the development of on-line instrumentation for the rapid detection of microorganisms in water supplies.
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Mori, Masanobu; Yamamoto, Tsukasa; Kaseda, Maki; Yamada, Sachiko; Itabashi, Hideyuki
2012-03-01
A combination of polyvinyl alcohol chemically coated capillary (PVA capillary) and background electrolyte (BGE) with ion-pair reagent (hexamethonium dichloride, HMC) was used on capillary ion electrophoresis-UV detection (CIE-UV) for analysis of Br⁻, I⁻, NO₂⁻, NO₃⁻, SCN⁻ and uric acid in human saliva. The PVA capillary prepared in our laboratory minimized electro-osmotic flow (EOF) at the BGE in pH 3-10, and did not affect the UV detection at 210 nm by the PVA-layer on capillary wall. Therefore, use of the PVA capillary was suitable for sensitive UV detection for analyte anions, as well as suppression of protein adsorption. In this study, we optimized the BGE of 10 mM phosphate plus 10 mM HMC with applying a voltage of -15 kV. HMC as an additive to BGE could manipulate the electrophoretic mobility of anions, without electrostatic adsorption to the PVA capillary. The CIE-UV could separate and determine analyte anions in human saliva containing proteins by the direct injection without pretreatments such as dilution or deproteinization within 13 min. The relative standard deviations (n=10) were ranged of 0.5-1.6% in migration times, 2.2-6.8% in peak heights and 2.8-8.4% in peak areas. The limits of detection (S/N=3) were ranged of 3.42-6.87 μM. The peak height of anions in this system was gradually decreased through the successive injections of saliva samples, but the problem was successfully solved by periodically conditioning the PVA capillary. The quantifiability of anions in human saliva samples by the CIE-UV was evaluated through the recoveries by standard addition methods and comparison of other representative analytical methods, as well as identification by ion chromatography (IC). From the anion analyses in 12 different saliva samples, the CIE-UV demonstrated that can obtain obvious differences in concentrations of SCN⁻ between of smoker and non-smoker and those of uric acid between male and female with satisfactory results. Copyright © 2012 Elsevier B.V. All rights reserved.
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Avula, Bharathi; Wang, Yan-Hong; Smillie, Troy J; Khan, Ikhlas A
2009-03-01
A UPLC-UV/ELSD method has been developed for analysis of major triterpenoids and formononetin in ACTAEA RACEMOSA L. (family Ranunculaceae) samples. The best results were obtained with an Acquity UPLC BEH C18 (100 mmx2.1 mm, i. d., 1 microm) column system using gradient elution with a mobile phase consisting of water and acetonitrile:methanol (7:3) at a constant flow rate of 0.3 mL/min. Owing to their low UV absorption, the triterpene saponins were detected by evaporative light scattering. Within 5.5 minutes, three main triterpenoid glycosides [cimiracemoside A, 23- EPI-26-deoxyactein, and actein] and an isoflavonoid, formononetin, could be separated, with detection limits of 5, 5, 10, and 0.01 microg/mL, respectively. The method was successfully used to analyze different Actaea racemosa market products as well as to distinguish between two other ACTAEA species. There was a significant variability in the amounts of the selected triterpene glycosides for the products containing black cohosh and rhizomes of black cohosh. The isoflavone formononetin was not detected in the samples analyzed. LC-MS coupled with the electrospray ionization (ESI) interface method is described for the identification of formononetin and triterpenoid glycosides in plant samples and dietary supplements that claim to contain black cohosh and different species of Actaea.
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Brünen, Sonja; Krüger, Ralf; Finger, Susann; Korf, Felix; Kiefer, Falk; Wiedemann, Klaus; Lackner, Karl J; Hiemke, Christoph
2010-02-01
We present data for a comparison of a liquid-chromatographic method coupled with tandem mass spectrometry (LC-MS/MS) and a high-performance liquid-chromatographic method with column switching and UV spectrophotometric detection. The two methods were developed for determination of naltrexone and 6beta-naltrexol in blood serum or plasma aiming to be used for therapeutic drug monitoring to guide the treatment of patients with naltrexone. For the high-performance liquid chromatography (HPLC)/UV detection, online sample cleanup was conducted on Perfect Bond C(18) material with 2% (vol/vol) acetonitrile in deionized water. Drugs were separated on a C(18) column using 11.5% (vol/vol) acetonitrile and 0.4% (vol/vol) N,N,N,N-tetramethylethylenediamine within 20 min. LC-MS/MS used naltrexone-d (3) and 6beta-naltrexol-d (4) as internal standards. After protein precipitation, the chromatographic separation was performed on a C(18) column by applying a methanol gradient (5-100%, vol/vol) with 0.1% formic acid over 9.5 min. The HPLC/UV method was found to be linear for concentrations ranging from 2 to 100 ng/ml, with a regression correlation coefficient of r (2) > 0.998 for naltrexone and 6beta-naltrexol. The limit of quantification was 2 ng/ml for naltrexone and 6beta-naltrexol. For the LC-MS/MS method the calibration curves were linear (r(2) > 0.999) from 0.5 to 200 ng/ml for both substances, and the limit of quantification was 0.5 ng/ml. The concentrations measured by the two methods correlated significantly for both substances (r(2) > 0.967; p < 0.001). Both methods could be used for therapeutic drug monitoring. The HPLC/UV method was advantageous regarding automatization and costs, whereas LC-MS/MS was superior with regard to sensitivity.
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Exploring Novel Spintronic Responses from Advanced Functional Organic Materials
2015-08-10
under 365 nm handheld UV lamp before (left) and after (right) writing letters with AA solution as ink. In summary, we could demonstrate a novel...to UV (360 nm) for 20 min, and the octadecyltrichlorosilane (OTS) treatment was carried out in an OTS vapor chamber (80 °C, vacuum, 2 h 30 min...serum to 20 mM in food and pharmaceuticals.5-7 A lot of analytical detection methods for AA have been developed including electrophoresis,8 UV -Vis
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Imamović, B; Sober, M; Becić, E
2009-10-01
The protection of sun radiation is a problem on global level for all living organisms on Earth. The need of people for the overexposure to the UV radiation led human population towards finding novel ways of protection of this kind of radiation, in form of cosmetic preparations applied on the skin. So far, the high values of protection factors of preparations and total block preparations with sun protection factor of 50+ were achieved. Physical and chemical filters which absorb radiation are constituents of these preparations. European Union has set regulations as which substances and in what amounts could be used as UV absorbers. American FDA (Food and Drug Administration) also gave its list of the most frequently used UV absorbers in the sunscreen products, as well as their declared concentrations. The most frequently used concentrations of UV filters in cosmetics is between 0.1% and 10%. Concentrations of UV filters in sunscreen products have to be monitored in order to ensure that they are not less from the declared levels, on which depends the efficacy and safety of the product. Butyl methoxydibenzoylmethane (BMDM) is used as a UV-A filter in suncare products. Optimized high performance liquid chromatography method for BMDM determination in the presence of other UV filters in suncare preparations is presented in this paper. Determination was performed on C(8) reversed phase using UV detection at 357 nm and isocratic mobile phase of acetonitrile and 0.5% phosphoric acid (70 : 30 v/v). Proposed method has limit of detection of 0.058 microg mL(-1), limit of quantification 0.193 microg mL(-1) and linearity correlation coefficient of 0.9989. Commercially available products were analysed using the proposed method. All analysed samples complied with EU directives limit of BMDM content to no more than 5%.
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Photochemical oxidation of persistent cyanide-related compounds
NASA Astrophysics Data System (ADS)
Budaev, S. L.; Batoeva, A. A.; Khandarkhaeva, M. S.; Aseev, D. G.
2017-03-01
Kinetic regularities of the photolysis of thiocyanate solutions using of mono- and polychromatic UV radiation sources with different spectral ranges are studied. Comparative experiments aimed at investigating the role of photochemical action during the oxidation of thiocyanates with persulfates and additional catalytic activation with iron(III) ions are performed. The rate of conversion and the initial rate of thiocyanate oxidation are found to change in the order UV < UV/S2O 8 2- < S2O 8 2- /Fe3+ < UV/S2O 8 2- /Fe3+. A synergistic effect is detected when using the combined catalytic method for the destruction of thiocyanates by the UV/S2O 8 2- /Fe3+ oxidation system. This effect is due to the formation of reactive oxygen species, as a result of both the decomposition of persulfate and the reduction of inactive Fe3+ intermediates into Fe3+.
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NASA Astrophysics Data System (ADS)
Ortega-Martinez, Antonio; Padilla-Martinez, Juan Pablo; Franco, Walfre
2016-04-01
The skin contains several fluorescent molecules or fluorophores that serve as markers of structure, function and composition. UV fluorescence excitation photography is a simple and effective way to image specific intrinsic fluorophores, such as the one ascribed to tryptophan which emits at a wavelength of 345 nm upon excitation at 295 nm, and is a marker of cellular proliferation. Earlier, we built a clinical UV photography system to image cellular proliferation. In some samples, the naturally low intensity of the fluorescence can make it difficult to separate the fluorescence of cells in higher proliferation states from background fluorescence and other imaging artifacts -- like electronic noise. In this work, we describe a statistical image segmentation method to separate the fluorescence of interest. Statistical image segmentation is based on image averaging, background subtraction and pixel statistics. This method allows to better quantify the intensity and surface distributions of fluorescence, which in turn simplify the detection of borders. Using this method we delineated the borders of highly-proliferative skin conditions and diseases, in particular, allergic contact dermatitis, psoriatic lesions and basal cell carcinoma. Segmented images clearly define lesion borders. UV fluorescence excitation photography along with statistical image segmentation may serve as a quick and simple diagnostic tool for clinicians.
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Optical spectrum of proflavine and its ions
NASA Astrophysics Data System (ADS)
Bonaca, A.; Bilalbegović, G.
2010-06-01
Motivated by possible astrophysical and biological applications we calculate visible and near UV spectral lines of proflavine (C13H11N3, 3,6-diaminoacridine) in vacuum, as well as its anion, cation, and dication. The pseudopotential density functional and time-dependent density functional methods are used. We find a good agreement in spectral line positions calculated by two real-time propagation methods and the Lanczos chain method. Spectra of proflavine and its ions show characteristic UV lines which are good candidates for a detection of these molecules in interstellar space and various biological processes.
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Lavigne, Claire; Durand, Gérard; Roblin, Antoine
2009-04-20
In the atmosphere pointlike sources are surrounded by an aureole due to molecular and aerosol scattering. UV phase functions of haze droplets have a very important forward peak that limits signal angular spreading in relation to the clear atmosphere case where Rayleigh scattering predominates. This specific property can be exploited using solar blind UV source detection as an aircraft landing aid under foggy conditions. Two methods have been used to compute UV light propagation, based on the Monte Carlo technique and a semi-empirical approach. Results obtained after addition of three types of sensor and UV runway light models show that an important improvement in landing conditions during foggy weather could be achieved by use of a solar blind UV intensified CCD camera with two stages of microchannel plates.
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Schulze, Philipp; Ludwig, Martin; Kohler, Frank; Belder, Detlev
2005-03-01
Deep UV fluorescence detection at 266-nm excitation wavelength has been realized for sensitive detection in microchip electrophoresis. For this purpose, an epifluorescence setup was developed enabling the coupling of a deep UV laser into a commercial fluorescence microscope. Deep UV laser excitation utilizing a frequency quadrupled pulsed laser operating at 266 nm shows an impressive performance for native fluorescence detection of various compounds in fused-silica microfluidic devices. Aromatic low molecular weight compounds such as serotonin, propranolol, a diol, and tryptophan could be detected at low-micromolar concentrations. Deep UV fluorescence detection was also successfully employed for the detection of unlabeled basic proteins. For this purpose, fused-silica chips dynamically coated with hydroxypropylmethyl cellulose were employed to suppress analyte adsorption. Utilizing fused-silica chips permanently coated with poly(vinyl alcohol), it was also possible to separate and detect egg white chicken proteins. These data show that deep UV fluorescence detection significantly widens the application range of fluorescence detection in chip-based analysis techniques.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Ganot, Noam; Gal-Yam, Avishay; Ofek, Eran O.
The radius and surface composition of an exploding massive star, as well as the explosion energy per unit mass, can be measured using early UV observations of core-collapse supernovae (SNe). We present the first results from a simultaneous GALEX/PTF search for early ultraviolet (UV) emission from SNe. Six SNe II and one Type II superluminous SN (SLSN-II) are clearly detected in the GALEX near-UV (NUV) data. We compare our detection rate with theoretical estimates based on early, shock-cooling UV light curves calculated from models that fit existing Swift and GALEX observations well, combined with volumetric SN rates. We find thatmore » our observations are in good agreement with calculated rates assuming that red supergiants (RSGs) explode with fiducial radii of 500 R{sub ⊙}, explosion energies of 10{sup 51} erg, and ejecta masses of 10 M{sub ⊙}. Exploding blue supergiants and Wolf–Rayet stars are poorly constrained. We describe how such observations can be used to derive the progenitor radius, surface composition, and explosion energy per unit mass of such SN events, and we demonstrate why UV observations are critical for such measurements. We use the fiducial RSG parameters to estimate the detection rate of SNe during the shock-cooling phase (<1 day after explosion) for several ground-based surveys (PTF, ZTF, and LSST). We show that the proposed wide-field UV explorer ULTRASAT mission is expected to find >85 SNe per year (∼0.5 SN per deg{sup 2}), independent of host galaxy extinction, down to an NUV detection limit of 21.5 mag AB. Our pilot GALEX/PTF project thus convincingly demonstrates that a dedicated, systematic SN survey at the NUV band is a compelling method to study how massive stars end their life.« less
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Analysis of penicillin G in milk by liquid chromatography.
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.
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den Brok, Monique W J; Nuijen, Bastiaan; Hillebrand, Michel J X; Grieshaber, Charles K; Harvey, Michael D; Beijnen, Jos H
2005-09-01
C1311 (5-[[2-(diethylamino)ethyl]amino]-8-hydroxyimidazo [4,5,1-de]-acridin-6-one-dihydrochloride trihydrate) is the lead compound from the group of imidazoacridinones, a novel group of rationally designed anticancer agents. The pharmaceutical development of C1311 necessitated the availability of an assay for the quantification and purity determination of C1311 active pharmaceutical ingredient (API) and its pharmaceutical dosage form. A reversed-phase liquid chromatographic method (RP-LC) with ultraviolet (UV) detection was developed, consisting of separation on a C18 column with phosphate buffer (60 mM; pH 3 with 1 M citric acid)-acetonitrile-triethylamine (83:17:0.05, v/v/v) as the mobile phase and UV-detection at 280 nm. The method was found to be linear over a concentration range of 2.50-100 microg/mL, precise and accurate. Accelerated stress testing showed degradation products, which were well separated from the parent compound, confirming its stability-indicating capacity. Moreover, the use of LC-MS and on-line photo diode array detection enabled us to propose structures for four degradation products. Two of these products were also found as impurities in the API and more abundantly in an impure lot of API.
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Anand, K; Singh, Thishana; Madhumitha, G; Phulukdaree, A; Gengan, Robert M; Chuturgoon, A A
2017-04-01
The bio-synthesized DTAuNPs have an average size of 21nm. The aggregation extent depends on the concentration of melamine, which was validated by UV-vis spectra and visual method of melamine detection was developed. The major observation in this method was the color change of DTAuNPs from red to purple due to the aggregation of ligand capped gold nanoparticles instigated by melamine. The reaction of color changes were processed due to the shifting of bonding in hydrogen in between nanoparticles and melamine. The aggregation extent depends on the concentration of melamine, which can be validated UV-vis spectra and visual method of detecting melamine is developed. The electron density and conventional UV-vis, FTIR spectroscopy and DFT studies on the ligand was performed using computational methods. The theoretical and experimental data for the energy transitions and the molar extinction coefficients of the ligands studied has been obtained. Further, the ligand capped gold nanoparticles was assessed for cytotoxicity against A549 cells which resulted in significant decrease in cell viability was noted in 50μg/mL DTAu, 4-ATP and AXT treated cells at 2h (85% and 66%) and 6h (83% and 36%) respectively, (p<0.01) were studied and reported in this manuscript. Copyright © 2017 Elsevier B.V. All rights reserved.
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Maher, Hadir M; Youssef, Rasha M; Khalil, Riad H; El-Bahr, Sabry M
2008-12-15
An efficient multiresidue method for the simultaneous determination of metronidazole (MET) and spiramycin (SPY) in tilapia fish muscle, based on high performance liquid chromatography with UV detection (HPLC-UV), has been developed. The drugs were extracted with 0.2% orthophosphoric acid-methanol (6:4), and the extracts were cleaned up on a solid phase extraction cartridge, C18 Sep-Pak light column. The LC separation was performed on a RP stainless-steel C-18 analytical column (150 mm x 4.6 mm, 5 microm) with a gradient elution system of 0.05 M phosphate buffer adjusted to pH 2.4-acetonitrile as the mobile phase at the flow rate of 1.0 ml min(-1). A wavelength programming was applied for the UV detection of the analytes. The method not only enabled the determination of the parent drugs, MET and SPY, but also permitted the determination of their metabolites, hydroxymetronidazole (HMET) and neospiramycin (NSPY). The calibration graphs for each drug were rectilinear in the range of 0.005-1.000 microg g(-1) for MET and HMET and 0.025-1.000 microg g(-1) for SPY and NSPY. With this method, the cited drugs with their metabolites were determined in fortified fish muscle tissues at levels of 0.025, 0.1 and 1.0 microg g(-1) with good accuracy and precision. LOD and LOQ obtained for each drug were as follows: 0.002 and 0.005 microg g(-1) for MET and HMET and 0.005 and 0.025 microg g(-1) for SPY and NSPY. Utilization of the method to successfully analyze tilapia fish muscle samples incurred with MET and SPY was described.
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Hügler, Michael; Böckle, Karin; Eberhagen, Ingrid; Thelen, Karin; Beimfohr, Claudia; Hambsch, Beate
2011-01-01
Monitoring of microbiological contaminants in water supplies requires fast and sensitive methods for the specific detection of indicator organisms or pathogens. We developed a protocol for the simultaneous detection of E. coli and coliform bacteria based on the Fluorescence in situ Hybridization (FISH) technology. This protocol consists of two approaches. The first allows the direct detection of single E. coli and coliform bacterial cells on the filter membranes. The second approach includes incubation of the filter membranes on a nutrient agar plate and subsequent detection of the grown micro-colonies. Both approaches were validated using drinking water samples spiked with pure cultures and naturally contaminated water samples. The effects of heat, chlorine and UV disinfection were also investigated. The micro-colony approach yielded very good results for all samples and conditions tested, and thus can be thoroughly recommended for usage as an alternative method to detect E. coli and coliform bacteria in water samples. However, during this study, some limitations became visible for the single cell approach. The method cannot be applied for water samples which have been disinfected by UV irradiation. In addition, our results indicated that green fluorescent dyes are not suitable to be used with chlorine disinfected samples.
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Mei, Meng; Huang, Xiaojia
2017-11-24
Due to the endocrine disrupting properties, organic UV filters have been a great risk for humans and other organisms. Therefore, development of accurate and effective analytical methods is needed for the determination of UV filters in environmental waters. In this work, a fast, sensitive and environmentally friendly method combining magnetism-enhanced monolith-based in-tube solid phase microextraction with high-performance liquid chromatography with diode array detection (DAD) (ME-MB-IT/SPME-HPLC-DAD) for the online analysis of five organic UV filters in environmental water samples was developed. To extract UV filters effectively, an ionic liquid-based monolithic capillary column doped with magnetic nanoparticles was prepared by in-situ polymerization and used as extraction medium of online ME-MB-IT/SPME-HPLC-DAD system. Several extraction conditions including the intensity of magnetic field, sampling and desorption flow rate, volume of sample and desorption solvent, pH value and ionic strength of sample matrix were optimized thoroughly. Under the optimized conditions, the extraction efficiencies for five organic UV filters were in the range of 44.0-100%. The limits of detection (S/N=3) and limits of quantification (S/N=10) were 0.04-0.26μg/L and 0.12-0.87μg/L, respectively. The precisions indicated by relative standard deviations (RSDs) were less than 10% for both intra- and inter-day variabilities. Finally, the developed method was successfully applied to the determination of UV filters in three environmental water samples and satisfactory results were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.
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NASA Astrophysics Data System (ADS)
Bradie, Johanna; Gianoli, Claudio; He, Jianjun; Lo Curto, Alberto; Stehouwer, Peter; Veldhuis, Marcel; Welschmeyer, Nick; Younan, Lawrence; Zaake, André; Bailey, Sarah
2018-03-01
Non-indigenous species seriously threaten native biodiversity. To reduce establishments, the International Maritime Organization established the Convention for the Control and Management of Ships' Ballast Water and Sediments which limits organism concentrations at discharge under regulation D-2. Most ships will comply by using on-board treatment systems to disinfect their ballast water. Port state control officers will need simple, rapid methods to detect compliance. Appropriate monitoring methods may be dependent on treatment type, since different treatments will affect organisms by a variety of mechanisms. Many indicative tools have been developed, but must be examined to ensure the measured variable is an appropriate signal for the response of the organisms to the applied treatment. We assessed the abilities of multiple analytic tools to rapidly detect the effects of a ballast water treatment system based on UV disinfection. All devices detected a large decrease in the concentrations of vital organisms ≥ 50 μm and organisms < 10 μm (mean 82.7-99.7% decrease across devices), but results were more variable for the ≥ 10 to < 50 μm size class (mean 9.0-99.9% decrease across devices). Results confirm the necessity to choose tools capable of detecting the damage inflicted on living organisms, as examined herein for UV-C treatment systems.
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AlKhalidi, Bashar A; Shtaiwi, Majed; AlKhatib, Hatim S; Mohammad, Mohammad; Bustanji, Yasser
2008-01-01
A fast and reliable method for the determination of repaglinide is highly desirable to support formulation screening and quality control. A first-derivative UV spectroscopic method was developed for the determination of repaglinide in tablet dosage form and for dissolution testing. First-derivative UV absorbance was measured at 253 nm. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ) in comparison to the U.S. Pharmacopeia (USP) column high-performance liquid chromatographic (HPLC) method. The first-derivative UV spectrophotometric method showed excellent linearity [correlation coefficient (r) = 0.9999] in the concentration range of 1-35 microg/mL and precision (relative standard deviation < 1.5%). The LOD and LOQ were 0.23 and 0.72 microg/mL, respectively, and good recoveries were achieved (98-101.8%). Statistical comparison of results of the first-derivative UV spectrophotometric and the USP HPLC methods using the t-test showed that there was no significant difference between the 2 methods. Additionally, the method was successfully used for the dissolution test of repaglinide and was found to be reliable, simple, fast, and inexpensive.
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Ceci, Edmondo; Montemurro, Nicola; Tantillo, Giuseppina; Di Pinto, Angela; Celano, Gaetano Vitale; Bozzo, Giancarlo
2014-01-01
The extensive use of pesticides in agriculture plays an important role in bees die-off and allows the presence of residues in hive products, particularly in honey. An accurate and reliable analytical method, based on QuEChERS extractive technique, has been developed for the quantitative determination by high-performance liquid chromatography UV-visible detector of 5 pesticides (Deltamethrin, Dimethoate, Imidacloprid, Acetamiprid, Chlorfenvinphos) in honey. The method, according to Commission Directive 2002/63/EC and Regulation 882/2004/EC, provided excellent results with respect to linearity (correlation coefficient up to 0.993), limits of detection and quantification (0.005 and 0.01 µg/mL for Dimethoate, Deltamethrin and Chlorfenvinphos; 0.02 and 0.05 µg/mL for Acetamiprid and Imidacloprid), recovery values (86.4 to 96.3%), precision and relative expanded uncertainty of a measurement, demonstrating the conformity of the this method with the European directives. The proposed method was applied to 23 samples of Apulian honey. None of the investigated pesticides was detected in these samples. PMID:27800334
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Peng, Li-Qing; Cao, Jun; Du, Li-Jing; Zhang, Qi-Dong; Shi, Yu-Tin; Xu, Jing-Jing
2017-05-26
An environmentally friendly ionic liquid-in-water (IL/W) microemulsion was established and applied as mobile phase in microemulsion liquid chromatography (MELC) with ultraviolet (UV) detection or electrochemical detector (ECD) for analysis of phenolic compounds in real samples. The optimal condition of the method was using the best composition of microemulsion (0.2% w/v [HMIM]PF 6 , 1.0% w/v SDS, 3.0% w/v n-butanol, 95.8% v/v water, pH 2.5) with UV detection. The validation results indicated that the method provided high degree of sensitivity, precision and accuracy with the low limit of detections ranged from 17.9-238ng/mL, satisfactory mean recovery values in the range of 80.1-105% and good linearity (r 2 >0.9994). Additionally, this method exhibited high selectivity and resolution for the analytes and was more eco-friendly compared with traditional MELC method. Consequently, the established IL/W MELC method was successfully applied to simultaneously separate and determine target compounds in Danshen sample and its preparation. Copyright © 2017 Elsevier B.V. All rights reserved.
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Gujral, Rajinder Singh; Haque, Sk Manirul
2010-01-01
A simple and sensitive UV spectrophotometric method was developed and validated for the simultaneous determination of Potassium Clavulanate (PC) and Amoxicillin Trihydrate (AT) in bulk, pharmaceutical formulations and in human urine samples. The method was linear in the range of 0.2–8.5 μg/ml for PC and 6.4–33.6 μg/ml for AT. The absorbance was measured at 205 and 271 nm for PC and AT respectively. The method was validated with respect to accuracy, precision, specificity, ruggedness, robustness, limit of detection and limit of quantitation. This method was used successfully for the quality assessment of four PC and AT drug products and in human urine samples with good precision and accuracy. This is found to be simple, specific, precise, accurate, reproducible and low cost UV Spectrophotometric method. PMID:23675211
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Avula, Bharathi; Wang, Yan-Hong; Smillie, Troy J; Mabusela, Wilfred; Vincent, Leszek; Weitz, Frans; Khan, Ikhlas A
2009-01-01
A simple and specific analytical method for the quantitative determination of flavonoids from the aerial parts of the Artemisia afra plant samples was developed. By column high-performance liquid chromatography (HPLC) with UV absorption and mass spectrometry (MS) detection, separation was achieved on a reversed-phase octadecylsilyl (C18) column with water, methanol, and acetonitrile, all containing 0.1% acetic acid, as the mobile phase. These methods were used to analyze various species of Artemisia plant samples. The wavelength used for quantification of flavonoids with the diode array detector was 335 nm. The limits of detection (LOD) by HPLC/MS were found to be 7.5, 7.5, 10, 2.0, and 2.0 ng/mL; and by LC-UV the LODs were 500, 500, 500, 300, and 300 ng/mL for apigenin, chrysoeriol, tamarixetin, acacetin, and genkwanin, respectively. The HPLC/MS method was found to be 50-150 times more sensitive than the HPLC-UV method. HPLC/MS coupled with an electrospray ionization interface is described for the identification and quantification of flavonoids in various plant samples. This method involved the use of the [M+H]+ ions of the compounds at mass-to-charge ratio of 1.0606, 301.0712, 317.0661, 285.0763, and 285.0763 (calculated mass), respectively, in the positive ion mode with extractive ion monitoring.
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Ford, Michael J; Deibel, Michael A; Tomkins, Bruce A; Van Berkel, Gary J
2005-07-15
Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 mum/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methods determined from the calibration curve statistics were 0.20 ng injected (0.50 muL) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by approximately 8% or more) than the literature values.
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Hernández-Borges, Javier; García-Montelongo, Francisco J; Cifuentes, Alejandro; Rodríguez-Delgado, Miguel Angel
2005-04-08
In this work, the combined use of solid-phase extraction (SPE) and on-line preconcentration strategies as normal stacking mode (NSM) and stacking with matrix removal (SWMR) for the ultrasensitive and simultaneous capillary electrophoresis-ultraviolet analysis (CE-UV) of five triazolopyrimidine sulfonanilide pesticides (i.e., diclosulam, cloransulam-methyl, flumetsulam, metosulam and florasulam) in different types of water is investigated. An adequate separation electrolyte for the separation and stacking of these pesticides was obtained, considering also its compatibility with MS detection, which consisted of 24 mM formic acid and 16 mM ammonium carbonate at pH 6.4. It was observed that the use of this running buffer together with the SWMR preconcentration method provided the best results in terms of sensitivity (between 6.54 and 11.9 microg/L) and peak efficiency (up to 550000 theoretical plates per meter, NTP/m). When this on-line preconcentration procedure was combined with an off-line sample preconcentration step as SPE using C18 cartridges, the selected herbicides could be detected in the ng/L range. The optimized SPE-SWMR-CE-UV method was applied to the determination of the selected group of pesticides in spiked and non-spiked mineral and stagnant waters. Recoveries ranged between 55 and 110% and limits of detection between 131 and 342 ng/L. This work shows the great possibilities of the combined use of SPE-SWMR-CE-UV to overcome the sensitivity problems usually linked to CE analysis.
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A simple method for plasma total vitamin C analysis suitable for routine clinical laboratory use.
Robitaille, Line; Hoffer, L John
2016-04-21
In-hospital hypovitaminosis C is highly prevalent but almost completely unrecognized. Medical awareness of this potentially important disorder is hindered by the inability of most hospital laboratories to determine plasma vitamin C concentrations. The availability of a simple, reliable method for analyzing plasma vitamin C could increase opportunities for routine plasma vitamin C analysis in clinical medicine. Plasma vitamin C can be analyzed by high performance liquid chromatography (HPLC) with electrochemical (EC) or ultraviolet (UV) light detection. We modified existing UV-HPLC methods for plasma total vitamin C analysis (the sum of ascorbic and dehydroascorbic acid) to develop a simple, constant-low-pH sample reduction procedure followed by isocratic reverse-phase HPLC separation using a purely aqueous low-pH non-buffered mobile phase. Although EC-HPLC is widely recommended over UV-HPLC for plasma total vitamin C analysis, the two methods have never been directly compared. We formally compared the simplified UV-HPLC method with EC-HPLC in 80 consecutive clinical samples. The simplified UV-HPLC method was less expensive, easier to set up, required fewer reagents and no pH adjustments, and demonstrated greater sample stability than many existing methods for plasma vitamin C analysis. When compared with the gold-standard EC-HPLC method in 80 consecutive clinical samples exhibiting a wide range of plasma vitamin C concentrations, it performed equivalently. The easy set up, simplicity and sensitivity of the plasma vitamin C analysis method described here could make it practical in a normally equipped hospital laboratory. Unlike any prior UV-HPLC method for plasma total vitamin C analysis, it was rigorously compared with the gold-standard EC-HPLC method and performed equivalently. Adoption of this method could increase the availability of plasma vitamin C analysis in clinical medicine.
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López-Montes, Ana; Blanc García, Rosario; Espejo, Teresa; Huertas-Perez, José F; Navalón, Alberto; Vílchez, José Luis
2007-04-01
A simple and rapid capillary electrophoretic method with UV detection (CE-UV) has been developed for the identification of five natural dyes namely, carmine, indigo, saffron, gamboge and Rubia tinctoria root. The separation was performed in a fused-silica capillary of 64.5 cm length and 50 microm id. The running buffer was 40 mM sodium tetraborate buffer solution (pH 9.25). The applied potential was 30 kV, the temperature was 25 degrees C and detections were performed at 196, 232, 252, 300 and 356 nm. The injections were under pressure of 50 mbar during 13 s. The method was applied to the identification of carminic acid, gambogic acid, crocetin, indigotin, alizarin and purpurin in the collection of drawings and maps at the Royal Chancellery Archives in Granada (Spain). The method was validated by using HPLC as a reference method.
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Xu, Limei; Zhang, Chongmiao; Xu, Pengcheng; Wang, Xiaochang C
2018-03-01
Traditional culture methods may underestimate the tolerance of microorganisms to disinfectants because of the existence of viable but nonculturable or sublethally injured cells after disinfection. The selection of a strict method is crucial for the evaluation of disinfection performance. The actions of 2 typical disinfectants - ultraviolet (UV) and chlorine - on the fecal indicator Escherichia coli were investigated by the detection of culturability, membrane permeability, metabolic activity, deoxyribonucleic acid (DNA), and messenger ribonucleic acid (mRNA). During UV disinfection, the irreversible damages in the cell membrane and cellular adenosine triphosphate (ATP) were negligible at low UV doses (<80mJ/cm 2 ). However, membrane permeability was damaged at low doses of chlorine (<5mg/L), leading to leakage of cellular ATP. Our study showed that a slight lesion in DNA was detected even at high doses of UV (400mJ/cm 2 ) and chlorine (>5mg/L) treatments. The decay of mRNA was more rapid than that of DNA. The degradation level of mRNA depended on the choice of target genes. After exposure to 50mJ/cm 2 UV dose or 5mg/L chlorine for 30min, the DNA damage repair function (RecA mRNA) was inhibited. The mRNA involved in the DNA damage repair function can be a potential indicator of bacterial viability. Copyright © 2017. Published by Elsevier B.V.
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Analysis of UV filters in tap water and other clean waters in Spain.
Díaz-Cruz, M Silvia; Gago-Ferrero, Pablo; Llorca, Marta; Barceló, Damià
2012-03-01
The present paper describes the development of a method for the simultaneous determination of five hormonally active UV filters namely benzophenone-3 (BP3), 3-(4-methylbenzylidene) camphor (4MBC), 2-ethylhexyl 4-(dimethylamino) benzoate (OD-PABA), 2-ethylhexyl 4-methoxycinnamate (EHMC) and octocrylene (OC) by means of solid-phase extraction and gas chromatography-electron impact ionization-mass spectrometry. Under optimized conditions, this methodology achieved low method limits of detection (needed for clean waters, especially drinking water analysis), between 0.02 and 8.42 ng/L, and quantitative recovery rates higher than 73% in all cases. Inter- and intraday precision for all compounds were lower than 7% and 11%, respectively. The optimized methodology was applied to perform the first survey of UV absorbing compounds in tap water from the metropolitan area and the city of Barcelona (Catalonia, Spain). In addition, other types of clean water matrices (mineral bottled water, well water and tap water treated with an ion-exchange resin) were investigated as well. Results evidenced that all the UV filters investigated were detected in the water samples analyzed. The compounds most frequently found were EHMC and OC. Maximum concentrations reached in tap water were 290 (BP3), 35 (4MBC), 110 (OD-PABA), 260 (EHMC), and 170 ng/L (OC). This study constitutes the first evidence of the presence of UV filter residues in tap water in Europe.
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UV spectroscopy determination of aqueous lead and copper ions in water
NASA Astrophysics Data System (ADS)
Tan, C. H.; Moo, Y. C.; Mat Jafri, M. Z.; Lim, H. S.
2014-05-01
Lead (Pb2+) and copper (Cu2+) ions are very common pollutants in water which have dangerous potential causing serious disease and health problems to human. The aim of this paper is to determine lead and copper ions in aqueous solution using direct UV detection without chemical reagent waste. This technique allow the determination of lead and copper ions from range 0.2 mg/L to 10 mg/L using UV wavelength from 205 nm to 225 nm. The method was successfully applied to synthetic sample with high performance.
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De Baere, S; Eeckhaut, V; Steppe, M; De Maesschalck, C; De Backer, P; Van Immerseel, F; Croubels, S
2013-06-01
A rapid and sensitive HPLC-UV method for the quantitative determination of four short-chain fatty acids (SCFAs) and lactic acid (LA) produced during in vitro fermentation is presented. Extraction of SCFAs from supernatants of bacterial cultures is aggravated due to their polarity and volatility. Detection can only be performed at a short, non-selective UV wavelength (210nm), due to the lack of any significant chromophore. Therefore special attention was paid to the optimization of the sample preparation procedure and the HPLC-UV conditions. The final extraction procedure consisted of a liquid-liquid back extraction using diethylether. Prior to HPLC-UV analysis the samples were acidified (pH<2) in order to improve retention of the SCFA's and LA on the Hypersil Gold aQ column. Matrix-matched calibration graphs were prepared for all analytes of interest (range 0.5-50mM) and correlation and goodness-of-fit coefficients were between 0.9951-0.9993 and 3.88-8.27%, respectively. Limits of detection and quantification ranged from 0.13 to 0.33mM and 0.5 to 1.0mM, respectively. The results for the within-day and between-day precision and accuracy fell within the ranges specified. The reported validated method has been successfully used for the in vitro screening of supernatants of bacterial cultures for the presence of butyric acid, aiming to select for butyric acid-producing bacteria. In addition, the method has been used to determine the production pattern of selected fatty acids by bacterial species isolated from human feces and chicken caeca. Copyright © 2013 Elsevier B.V. All rights reserved.
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Beeman, Michael G; Nze, Ugochukwu C; Sant, Himanshu J; Malik, Hammad; Mohanty, Swomitra; Gale, Bruce K; Carlson, Krista
2018-05-10
The availability of clean drinking water is a significant problem worldwide. Many technologies exist for purifying drinking water, however, many of these methods require chemicals or use simple methods, such as boiling and filtering, which may or may not be effective in removing waterborne pathogens. Present methods for detecting pathogens in point-of-use (POU) sterilized water are typically time prohibitive or have limited ability differentiating between active and inactive cells. This work describes a rapid electrochemical sensor to differentially detect the presence of active Escherichia coli (E. coli) O157:H7 in samples that have been partially or completely sterilized using a new POU electrocatalytic water purification technology based on superradicals generated by defect laden titania (TiO₂) nanotubes. The sensor was also used to detect pathogens sterilized by UV-C radiation for a comparison of different modes of cell death. The sensor utilizes immunomagnetic bead separation to isolate active bacteria by forming a sandwich assay comprised of antibody functionalized secondary magnetic beads, E. coli O157:H7, and polyguanine (polyG) oligonucleotide functionalized secondary polystyrene beads as an electrochemical tag. The assay is formed by the attachment of antibodies to active receptors on the membrane of E. coli , allowing the sensor to differentially detect viable cells. Ultravioloet (UV)-C radiation and an electrocatalytic reactor (ER) with integrated defect-laden titania nanotubes were used to examine the sensors’ performance in detecting sterilized cells under different modes of cell death. Plate counts and flow cytometry were used to quantify disinfection efficacy and cell damage. It was found that the ER treatments shredded the bacteria into multiple fragments, while UV-C treatments inactivated the bacteria but left the cell membrane mostly intact.
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Filho, Adalberto M; dos Santos, Fábio N; Pereira, Pedro A de Paula
2011-11-01
A sensitive and efficient solid-phase microextraction method, based on liquid chromatography and UV-Vis detection, was developed and validated as an alternative method for sample screening prior to LC-MS analysis. It enables the simultaneous determination of ten pesticides in mango fruits. The fiber used was polydimethylsiloxane while optimum SPME conditions employed have been developed and optimized in a previous work. The desorption process was performed in static mode, using acetonitrile as a solvent. The results indicate that the DI-SPME/HPLC/UV-Vis procedure resulted in good linear range, accuracy, precision and sensibility and is adequate for analyzing pesticide residues in mango fruits. The limits of detection (0.6-3.3 μg/kg) and quantification (2.0-10.0 μg/kg) were achieved with values lower than the maximum residue levels (MRLs) established by Brazilian legislation for all pesticides in this study. The average recovery rates obtained for each pesticide ranged from 71.6 to 104.3% at three fortification levels, with the relative standard deviation ranging from 4.3 to 18.6%. The proposed method was applied for the determination of the aforementioned compounds in commercial mango samples and residues of azoxystrobin, fenthion, permethrin, abamectin and bifenthrin were detected in the mango samples, although below the MRLs established by Brazilian legislation. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Chuanxiang, Wu; Lian, Xia; Lijie, Liu; Fengli, Qu; Zhiwei, Sun; Xianen, Zhao; Jinmao, You
2016-02-01
A sensitive and efficient method of high performance liquid chromatography using 1-(2-naphthyl)-3-methyl-5-pyrazolone (NMP) as pre-column derivatization reagent coupled with UV detection (HPLC-UV) and online mass spectrometry identification was established for determination of the most common N-Acetylhexosamines (N-acetyl-d-glucosamine (GlcNAc) and N-acetyl-d-galactosamine (GalNAc)) and N-acetylneuraminic acid (Neu5Ac). In order to obtain the highest liberation level of the three monosaccharides without destruction of Neu5Ac or conversion of GlcNAc/GalNAc to GlcN/GalN in the hydrolysis procedure, the pivotal parameters affecting the liberation of N-acetylhexosamines/Neu5Ac from sample were investigated with response surface methodology (RSM). Under the optimized condition, maximum yield was obtained. The effects of key parameters on derivatization, separation and detection were also investigated. At optimized conditions, three monosaccharides were labeled fast and entirely, and all derivatives exhibited a good baseline resolution and high detection sensitivity. The developed method was linear over the calibration range 0.25-12μM, with R(2)>0.9991. The detection limits of the method were between 0.48 and 2.01pmol. Intra- and inter-day precisions for the three monosaccharides (GlcNAc, GalNAc and Neu5Ac) were found to be in the range of 3.07-4.02% and 3.69-4.67%, respectively. Individual monosaccharide recovery from spiked milk was in the range of 81%-97%. The sensitivity of the method, the facility of the derivatization procedure and the reliability of the hydrolysis conditions suggest the proposed method has a high potential for utilization in routine trace N-acetylhexosamines and Neu5Ac analysis in biological samples. Copyright © 2015 Elsevier B.V. All rights reserved.
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A newly developed integrated cell culture reverse transcriptase quantitative PCR (ICC-RTqPCR) method and its applicability in UV disinfection studies is described. This method utilizes a singular cell culture system coupled with four RTqPCR assays to detect infectious serotypes t...
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Colorimetric As (V) detection based on S-layer functionalized gold nanoparticles.
Lakatos, Mathias; Matys, Sabine; Raff, Johannes; Pompe, Wolfgang
2015-11-01
Herein, we present simple and rapid colorimetric and UV/VIS spectroscopic methods for detecting anionic arsenic (V) complexes in aqueous media. The methods exploit the aggregation of S-layer-functionalized spherical gold nanoparticles of sizes between 20 and 50 nm in the presence of arsenic species. The gold nanoparticles were functionalized with oligomers of the S-layer protein of Lysinibacillus sphaericus JG-A12. The aggregation of the nanoparticles results in a color change from burgundy-red for widely dispersed nanoparticles to blue for aggregated nanoparticles. A detailed signal analysis was achieved by measuring the shift of the particle plasmon resonance signal with UV/VIS spectroscopy. To further improve signal sensitivity, the influence of larger nanoparticles was tested. In the case of 50 nm gold nanoparticles, a concentration of the anionic arsenic (V) complex lower than 24 ppb was detectable. Copyright © 2015 Elsevier B.V. All rights reserved.
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Asea, P A; Patterson, J R; Korsrud, G O; Dowling, P M; Boison, J O
2001-01-01
A new and sensitive liquid chromatography-ultra violet method with a detection limit of 6 ng/g (ppb) and a limit of quantification of 15 ng/g was developed for the determination of flunixin residues in bovine muscle tissue. Flunixin in homogenized animal tissue was extracted with acetonitrile after enzyme digestion. The tissue digest (extract) was then cleaned up on a solid-phase extraction cartridge and eluted with acidified hexane. After the eluate was evaporated to dryness under nitrogen at 55 degrees C, the residue was reconstituted in 1 mL mobile phase solution and analyzed by reversed-phase gradient chromatography with UV detection at 285 nm. The method was then applied in a survey study of slaughter animals to determine whether flunixin is being used in an off-label manner for veal and beef production in Canada.
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Uric acid detection using uv-vis spectrometer
NASA Astrophysics Data System (ADS)
Norazmi, N.; Rasad, Z. R. Abdul; Mohamad, M.; Manap, H.
2017-10-01
The aim of this research is to detect uric acid (UA) concentration using Ultraviolet-Visible (UV-Vis) spectrometer in the Ultraviolet (UV) region. Absorption technique was proposed to detect different uric acid concentrations and its UV absorption wavelength. Current practices commonly take a lot of times or require complicated structures for the detection process. By this proposed spectroscopic technique, every concentration can be detected and interpreted into an absorbance value at a constant wavelength peak in the UV region. This is due to the chemical characteristics belong to the uric acid since it has a particular absorption cross-section, σ which can be calculated using Beer’s Lambert law formula. The detection performance was displayed using Spectrasuite sofware. It showed fast time response about 3 seconds. The experiment proved that the concentrations of uric acid were successfully detected using UV-Vis spectrometer at a constant absorption UV wavelength, 294.46 nm in a low time response. Even by an artificial sample of uric acid, it successfully displayed a close value as the ones reported with the use of the medical sample. It is applicable in the medical field and can be implemented in the future for earlier detection of abnormal concentration of uric acid.
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77 FR 67282 - Dinotefuran; Pesticide Tolerances for Emergency Exemptions
Federal Register 2010, 2011, 2012, 2013, 2014
2012-11-09
... performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) method is available. For the determination of residues of dinotefuran only, an HPLC/ultraviolet (UV) detection method is available. For the determination of only the metabolites (DN and UF), HPLC/MS and HPLC/MS/MS methods are available. These methods...
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Detection of elemental mercury by multimode diode laser correlation spectroscopy.
Lou, Xiutao; Somesfalean, Gabriel; Svanberg, Sune; Zhang, Zhiguo; Wu, Shaohua
2012-02-27
We demonstrate a method for elemental mercury detection based on correlation spectroscopy employing UV laser radiation generated by sum-frequency mixing of two visible multimode diode lasers. Resonance matching of the multimode UV laser is achieved in a wide wavelength range and with good tolerance for various operating conditions. Large mode-hops provide an off-resonance baseline, eliminating interferences from other gas species with broadband absorption. A sensitivity of 1 μg/m3 is obtained for a 1-m path length and 30-s integration time. The performance of the system shows promise for mercury monitoring in industrial applications.
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Syed, Haroon Khalid; Liew, Kai Bin; Loh, Gabriel Onn Kit; Peh, Kok Khiang
2015-03-01
A stability-indicating HPLC-UV method for the determination of curcumin in Curcuma longa extract and emulsion was developed. The system suitability parameters, theoretical plates (N), tailing factor (T), capacity factor (K'), height equivalent of a theoretical plate (H) and resolution (Rs) were calculated. Stress degradation studies (acid, base, oxidation, heat and UV light) of curcumin were performed in emulsion. It was found that N>6500, T<1.1, K' was 2.68-3.75, HETP about 37 and Rs was 1.8. The method was linear from 2 to 200 μg/mL with a correlation coefficient of 0.9998. The intra-day precision and accuracy for curcumin were ⩽0.87% and ⩽2.0%, while the inter-day precision and accuracy values were ⩽2.1% and ⩽-1.92. Curcumin degraded in emulsion under acid, alkali and UV light. In conclusion, the stability-indicating method could be employed to determine curcumin in bulk and emulsions. Copyright © 2014 Elsevier Ltd. All rights reserved.
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Pól, Jaroslav; Varadová Ostrá, Elena; Karásek, Pavel; Roth, Michal; Benesová, Karolínka; Kotlaríková, Pavla; Cáslavský, Josef
2007-08-01
Pressurised fluid extraction using water or methanol was employed for the extraction of stevioside from Stevia rebaudiana Bertoni. The extraction method was optimised in terms of temperature and duration of the static or the dynamic step. Extracts were analysed by liquid chromatography followed by UV and mass-spectrometric (MS) detections. Thermal degradation of stevioside was the same in both solvents within the range 70-160 degrees C. Methanol showed better extraction ability for isolation of stevioside from Stevia rebaudiana leaves than water within the range 110-160 degrees C. However, water represents the green alternative to methanol. The limit of detection of stevioside in the extract analysed was 30 ng for UV detection and 2 ng for MS detection.
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Altiokka, G; Atkosar, Z; Can, N O
2002-10-15
A flow injection analysis (FIA) using UV detection, potentiometry and conductometry for levofloxacin (LVF) are described in this study. The best solvent system was found to consist of 0.2 M acetate buffer at pH 3 having 10% MeOH. A flow rate of 1 ml min(-1) was pumped and active material was detected at 288 nm. The detection limit (LOD) and limit of quantification (LOQ) for FIA were calculated to be 3 x 10(-7) M (S/N = 3) and 1 x 10(-7) M (S/N = 10), respectively. In the analysis of tablets, the RSD values were found to be 0.83, 0.98 and 0.99 for FIA, potentiometric and conductometric methods, respectively. Copyright 2002 Elsevier Science B.V.
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Analytical Stability-Indicating Methods for Alogliptin in Tablets by LC-CAD and LC-UV.
Bertol, Charise Dallazem; Friedrich, Maria Tereza; Carlos, Graciela; Froehlich, Pedro Eduardo
2017-03-01
Stability-indicating LC methods using a UV detector and a charged aerosol detector (CAD) simultaneously were validated for the assessment of alogliptin (ALG) in tablets. The analysis was performed on a C8 column (250 × 4.6 mm, 5 μm) at a flow of 0.8 mL/min, using acetonitrile-10 mM ammonium acetate buffer (pH 3.5; 90 + 10, v/v) as mobile phase and UV detection at 275 nm. Validation followed the International Conference on Harmonization guidelines. The method was linear over the range of 25-200 μg/mL. Normality of the residuals showed a normal distribution, no autocorrelation, and homoscedasticity. LODs were 6.25 and 2.65 µg/mL and LOQs were 20.85 and 8.84 µg/mL for the CAD and the UV detector, respectively. The methods were precise and accurate. Excipients and degradation products did not interfere in the methods in studies of specificity. None of the factors studied in the analysis of robustness had a significant effect on the quantification of the ALG by the Pareto chart. The results of the assay obtained with LC-CAD and LC-UV were similar. The methods could be considered interchangeable and stability-indicating, and can be applied as an appropriate QC tool for analysis of ALG in tablets.
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Liang, Jing; Wang, Qiuquan; Huang, Benli
2005-01-01
An online UV photolysis and UV/TiO2 photocatalysis reduction device (UV-UV/TiO2 PCRD) and an electrochemical vapor generation (ECVG) cell have been used for the first time as an interface between high-performance liquid chromatography (HPLC) and atomic fluorescence spectrometry (AFS) for selenium speciation. The newly designed ECVG cell of approximately 115 microL dead volume consists of a carbon fiber cathode and a platinum loop anode; the atomic hydrogen generated on the cathode was used to reduce selenium to vapor species for AFS determination. The noise was greatly reduced compared with that obtained by use of the UV-UV/TiO2 PCRD-KBH4-acid interface. The detection limits obtained for seleno-DL: -cystine (SeCys), selenite (Se(IV)), seleno-DL: -methionine (SeMet), and selenate (Se(VI)) were 2.1, 2.9, 4.3, and 3.5 ng mL(-1), respectively. The proposed method was successfully applied to the speciation of selenium in water-soluble extracts of garlic shoots cultured with different selenium species. The results obtained suggested that UV-UV/TiO2 PCRD-ECVG should be an effective interface between HPLC and AFS for the speciation of elements amenable to vapor generation, and is superior to methods involving KBH4.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Ford, Michael J; Deibel, Michael A.; Tomkins, Bruce A
Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methodsmore » determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.« less
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Nandre, Jitendra P; Patil, Samadhan R; Sahoo, Suban K; Pradeep, Chullikkattil P; Churakov, Andrei; Yu, Fabiao; Chen, Lingxin; Redshaw, Carl; Patil, Ashok A; Patil, Umesh D
2017-10-24
The pyridine substituted thiourea derivative PTB-1 was synthesized and characterized by spectroscopic techniques as well as by single crystal X-ray crystallography. The metal ion sensing ability of PTB-1 was explored by various experimental (naked-eye, UV-Vis, fluorescence, mass spectrometry and 1 H NMR spectroscopy) and theoretical (B3LYP/6-31G**/LANL2DZ) methods. PTB-1 exhibited a highly selective naked-eye detectable color change from colorless to dark brown and UV-Vis spectral changes for the detection of Ag + with a detection limit of 3.67 μM in aqueous medium. The detection of Ag + ions was achieved by test paper strip and supported silica methods. In contrast, PTB-1 exhibited a 23-fold enhanced emission at 420 nm in the presence of Hg 2+ ions with a nano-molar detection limit of 0.69 nM. Finally, the sensor PTB-1 was applied successfully for the intracellular detection of Hg 2+ ions in a HepG2 liver cell line, which was monitored by the use of confocal imaging techniques.
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Bahrani, Sonia; Ghaedi, Mehrorang; Khoshnood Mansoorkhani, Mohammad Javad; Ostovan, Abbas
2017-01-01
A selective and rapid method was developed for quantification of curcumin in human plasma and food samples using molecularly imprinted magnetic multiwalled carbon nanotubes (MMWCNTs) which was characterized with EDX and FESEM. The role of sorbent mass, volume of eluent and sonication time on response in solid phase microextraction procedure were optimized by central composite design (CCD) combined with response surface methodology (RSM) using Statistica. Preliminary experiments reveal that among different solvents, methanol:dimethyl sulfoxide (4:1V/V) led to efficient and quantitative elution of analyte. A reversed-phase high performance liquid chromatographic technique with UV detection (HPLC-UV) was applied for detection of curcumin content. The assay procedure involves chromatographic separation on analytical Nucleosil C18 column (250×4.6mm I.D., 5μm particle size) at ambient temperature with acetonitrile-water adjusted at pH=4.0 (20:80, v/v) as mobile phase at flow rate of 1.0mLmin -1 , while UV detector was set at 420nm. Under optimized conditions, the method demonstrated linear calibration curve with good detection limit (0.028ngmL -1 ) and R 2 =0.9983. The proposed method was successfully applied to biological fluid and food samples including ginger powder, curry powder, and turmeric powder. Copyright © 2016. Published by Elsevier B.V.
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Kim, Ho Jin
2016-01-01
A novel and simple method for detecting six water-soluble vitamins in animal feed using high performance liquid chromatography equipped with a photodiode array detector (HPLC/PDA) and ion-pairing reagent was developed. The chromatographic peaks of the six water-soluble vitamins were successfully identified by comparing their retention times and UV spectra with reference standards. The mobile phase was composed of buffers A (5 mM PICB-6 in 0.1% CH3COOH) and B (5 mM PICB-6 in 65% methanol). All peaks were detected using a wavelength of 270 nm. Method validation was performed in terms of linearity, sensitivity, selectivity, accuracy, and precision. The limits of detection (LODs) for the instrument employed in these experiments ranged from 25 to 197 μg/kg, and the limits of quantification (LOQs) ranged from 84 to 658 μg/kg. Average recoveries of the six water-soluble vitamins ranged from 82.3% to 98.9%. Method replication resulted in intraday and interday peak area variation of <5.6%. The developed method was specific and reliable and is therefore suitable for the routine analysis of water-soluble vitamins in animal feed.
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Effects of Regolith Properties on UV/VIS Spectra and Implications for Lunar Remote Sensing
NASA Astrophysics Data System (ADS)
Coman, Ecaterina Oana
Lunar regolith chemistry, mineralogy, various maturation factors, and grain size dominate the reflectance of the lunar surface at ultraviolet (UV) to visible (VIS) wavelengths. These regolith properties leave unique fingerprints on reflectance spectra in the form of varied spectral shapes, reflectance intensity values, and absorption bands. With the addition of returned lunar soils from the Apollo and Luna missions as ground truth, these spectral fingerprints can be used to derive maps of global lunar chemistry or mineralogy to analyze the range of basalt types on the Moon, their spatial distribution, and source regions for clues to lunar formation history and evolution. The Lunar Reconnaissance Orbiter Camera (LROC) Wide Angle Camera (WAC) is the first lunar imager to detect bands at UV wavelengths (321 and 360 nm) in addition to visible bands (415, 566, 604, 643, and 689 nm). This dissertation uses a combination of laboratory and remote sensing studies to examine the relation between TiO2 concentration and WAC UV/VIS spectral ratios and to test the effects of variations in lunar chemistry, mineralogy, and soil maturity on ultraviolet and visible wavelength reflectance. Chapter 1 presents an introduction to the dissertation that includes some background in lunar mineralogy and remote sensing. Chapter 2 covers coordinated analyses of returned lunar soils using UV-VIS spectroscopy, X-ray diffraction, and micro X-ray fluorescence. Chapter 3 contains comparisons of local and global remote sensing observations of the Moon using LROC WAC and Clementine UVVIS TiO2 detection algorithms and Lunar Prospector (LP) Gamma Ray Spectrometer (GRS)-derived FeO and TiO2 concentrations. While the data shows effects from maturity and FeO on the UV/VIS detection algorithm, a UV/VIS relationship remains a simple yet accurate method for TiO2 detection on the Moon.
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Liu, Jinmei; Wu, Weiwei; Bai, Suo; Qin, Yong
2011-11-01
Well aligned ZnO nanowire (NW) arrays are grown on Kevlar fiber and Kapton film via the chemical vapor deposition (CVD) method. These NWs have better crystallinity than those synthesized through the low-temperature hydrothermal method. The average length and diameter of ZnO NWs grown on Kevlar fiber can be controlled from 0.5 to 2.76 μm and 30 to 300 nm, respectively. A flexible ultraviolet (UV) sensor based on Kevlar fiber/ZnO NWs hybrid structure is made to detect UV illumination quantificationally.
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Çelik, S Esin; Özyürek, Mustafa; Güçlü, Kubilay; Çapanoğlu, Esra; Apak, Reşat
2014-01-01
Development and application of an on-line cupric reducing anti-oxidant capacity (CUPRAC) assay coupled with HPLC for separation and on-line determination of phenolic anti-oxidants in elderflower (Sambucus nigra L.) extracts for their anti-oxidant capacity are significant for evaluating health-beneficial effects. Moreover, this work aimed to assay certain flavonoid glycosides of elderflower that could not be identified/quantified by other similar on-line HPLC methods (i.e. 2,2-diphenyl-1-picrylhdrazyl and 2, 2'-azino-bis-3-ethylbenzothiazoline-6-sulphonic acid). To identify anti-oxidant constituents in elderflower by HPLC and to evaluate their individual anti-oxidant capacities by on-line HPLC-CUPRAC assay with a post-column derivatisation system. The separation and UV detection of polyphenols were performed on a C18 -column using gradient elution with two different mobile phase solutions, that is acetonitrile and 1% glacial acetic acid, with detection at 340 nm. The HPLC-separated anti-oxidant polyphenols in column effluent react with copper(II)-neocuproine in a reaction-coil to reduce the latter to copper(I)-neocuproine (Cu(I)-Nc) chelate having maximum absorption at 450 nm. The detection limits of tested compounds at 450 nm after post-column derivatisation were compared with those of at 340 nm UV-detection without derivatisation. LOD values (µg/mL) of quercetin and its glycosides at 450 nm were lower than those of UV detection at 340 nm. This method was applied successfully to elderflower extract. The flavonol glycosides of quercetin and kaempferol bound to several sugar components (glucose, rhamnose, galactose and rutinose) were identified in the sample. The on-line HPLC-CUPRAC method was advantageous over on-line ABTS and DPPH methods for measuring the flavonoid glycosides of elderflower. Copyright © 2014 John Wiley & Sons, Ltd.
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NASA Astrophysics Data System (ADS)
Rohyami, Yuli; Pribadi, Rizki Maulana
2017-12-01
Formalin is a food preservative that is prohibited by the government, but the abuse of these chemicals is still widely found. The presence of formalin can be detected by using a typical reagent that can ensure the presence of formaldehyde qualitatively and quantitatively. This research was conducted to validate the method of determining formalin in tofu by using Nash reagent in UV-Vis spectrophotometry. The addition of Nash reagent will lead to the formation of diacetyldihydrolutidin complex. The study was performed by stability test of deacetyldihydrolutidine complex against time and pH. Validation of methods for formalin testing in tofu with diacetyldihydrolutidine by UV-Vis spectrophotometry. The results showed that 3,5-diacetyl-dihydrolutidine complex is stable at pH of 7 and stable in the range of 70-120 minutes. The validation shows that the method gives good precision and accuracy of 83.78%. The method has the limit of detection of 1.3681 µg/mL, limit of quantification of 4,5603 µg/mL, and the estimated uncertainty of measurement of 1.30 µg/mL. The test showed that the tofu contained formalin 3.09 ± 1.30 µg/mL. These values provide information that this method can be used as a procedure for the determination of formalin on tofu.
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El-Gindy, Alaa; Emara, Samy; Shaaban, Heba
2007-02-19
Three methods are developed for the determination of two multicomponent mixtures containing guaiphenesine (GU) with salbutamol sulfate (SL), methylparaben (MP) and propylparaben (PP) [mixture 1]; and acephylline piperazine (AC) with bromhexine hydrochloride (BX), methylparaben (MP) and propylparaben (PP) [mixture 2]. The resolution of the two multicomponent mixtures has been accomplished by using numerical spectrophotometric methods such as partial least squares (PLS-1) and principal component regression (PCR) applied to UV absorption spectra of the two mixtures. In addition HPLC method was developed using a RP 18 column at ambient temperature with mobile phase consisting of acetonitrile-0.05 M potassium dihydrogen phosphate, pH 4.3 (60:40, v/v), with UV detection at 243 nm for mixture 1, and mobile phase consisting of acetonitrile-0.05 M potassium dihydrogen phosphate, pH 3 (50:50, v/v), with UV detection at 245 nm for mixture 2. The methods were validated in terms of accuracy, specificity, precision and linearity in the range of 20-60 microg ml(-1) for GU, 1-3 microg ml(-1) for SL, 20-80 microg ml(-1) for AC, 0.2-1.8 microgml(-1) for PP and 1-5 microg ml(-1) for BX and MP. The proposed methods were successfully applied for the determination of the two multicomponent combinations in laboratory prepared mixtures and commercial syrups.
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NASA Astrophysics Data System (ADS)
Mironov, Gleb G.; Logie, Jennifer; Okhonin, Victor; Renaud, Justin B.; Mayer, Paul M.; Berezovski, Maxim V.
2012-07-01
We present affinity capillary electrophoresis and mass spectrometry (ACE-MS) as a comprehensive separation technique for label-free solution-based affinity analysis. The application of ACE-MS for measuring affinity constants between eight small molecule drugs [ibuprofen, s-flurbiprofen, diclofenac, phenylbutazone, naproxen, folic acid, resveratrol, and 4,4'-(propane-1,3-diyl) dibenzoic acid] and β-cyclodextrin is described. We couple on-line ACE with MS to combine the separation and kinetic capability of ACE together with the molecular weight and structural elucidation of MS in one system. To understand the full potential of ACE-MS, we compare it with two other methods: Direct infusion mass spectrometry (DIMS) and ACE with UV detection (ACE-UV). After the evaluation, DIMS provides less reliable equilibrium dissociation constants than separation-based ACE-UV and ACE-MS, and cannot be used solely for the study of noncovalent interactions. ACE-MS determines apparent dissociation constants for all reacting small molecules in a mixture, even in cases when drugs overlap with each other during separation. The ability of ACE-MS to interact, separate, and rapidly scan through m/z can facilitate the simultaneous affinity analysis of multiple interacting pairs, potentially leading to the high-throughput screening of drug candidates.
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Fabricating a UV-Vis and Raman Spectroscopy Immunoassay Platform.
Hanson, Cynthia; Israelsen, Nathan D; Sieverts, Michael; Vargis, Elizabeth
2016-11-10
Immunoassays are used to detect proteins based on the presence of associated antibodies. Because of their extensive use in research and clinical settings, a large infrastructure of immunoassay instruments and materials can be found. For example, 96- and 384-well polystyrene plates are available commercially and have a standard design to accommodate ultraviolet-visible (UV-Vis) spectroscopy machines from various manufacturers. In addition, a wide variety of immunoglobulins, detection tags, and blocking agents for customized immunoassay designs such as enzyme-linked immunosorbent assays (ELISA) are available. Despite the existing infrastructure, standard ELISA kits do not meet all research needs, requiring individualized immunoassay development, which can be expensive and time-consuming. For example, ELISA kits have low multiplexing (detection of more than one analyte at a time) capabilities as they usually depend on fluorescence or colorimetric methods for detection. Colorimetric and fluorescent-based analyses have limited multiplexing capabilities due to broad spectral peaks. In contrast, Raman spectroscopy-based methods have a much greater capability for multiplexing due to narrow emission peaks. Another advantage of Raman spectroscopy is that Raman reporters experience significantly less photobleaching than fluorescent tags 1 . Despite the advantages that Raman reporters have over fluorescent and colorimetric tags, protocols to fabricate Raman-based immunoassays are limited. The purpose of this paper is to provide a protocol to prepare functionalized probes to use in conjunction with polystyrene plates for direct detection of analytes by UV-Vis analysis and Raman spectroscopy. This protocol will allow researchers to take a do-it-yourself approach for future multi-analyte detection while capitalizing on pre-established infrastructure.
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Giovannelli, D; Abballe, F
2005-08-26
A method has been developed which allows simultaneous determination of three linear alkyl trimethylammonium salts. Dodecyltrimethylammonium chloride, tetradecyltrimethylammonium bromide and hexadecyltrimethylammonium chloride are widely used as main active ingredients of lysing reagents for blood cell analyzers which perform white blood cells differential determination into two or more sub-populations by impedance analysis. The ion-pair on styrene-divinyl benzene chromatographic phase looks like a suitable, reliable and long term stable tool for separation of such quaternary compounds. The detection based on suppressed conductivity was chosen because of the lack of significance chromophores. A micromembrane suppressor device compatible with high solvent concentration (up to 80%) was used in order to minimize the conductivity background before the detection. In the present work we show how the chemical post column derivatization makes the alkyl chain detectable also by UV direct detection at 210 nm.
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Zuway, Khaled Y; Smith, Jamie P; Foster, Christopher W; Kapur, Nikil; Banks, Craig E; Sutcliffe, Oliver B
2015-09-21
The global increase in the production and abuse of cathinone-derived New Psychoactive Substances (NPSs) has developed the requirement for rapid, selective and sensitive protocols for their separation and detection. Electrochemical sensing of these compounds has been demonstrated to be an effective method for the in-field detection of these substances, either in their pure form or in the presence of common adulterants, however, the technique is limited in its ability to discriminate between structurally related cathinone-derivatives (for example: (±)-4′-methylmethcathinone (4-MMC, 2a) and (±)-4′-methyl-N-ethylmethcathinone (4-MEC, 2b) when they are both present in a mixture. In this paper we demonstrate, for the first time, the combination of HPLC-UV with amperometric detection (HPLC-AD) for the qualitative and quantitative analysis of 4-MMC and 4-MEC using either a commercially available impinging jet (LC-FC-A) or custom-made iCell channel (LC-FC-B) flow-cell system incorporating embedded graphite screen-printed macroelectrodes. The protocol offers a cost-effective, reproducible and reliable sensor platform for the simultaneous HPLC-UV and amperometric detection of the target analytes. The two systems have similar limits of detection, in terms of amperometric detection [LC-FC-A: 14.66 μg mL(-1) (2a) and 9.35 μg mL(-1) (2b); LC-FC-B: 57.92 μg mL(-1) (2a) and 26.91 μg mL(-1) (2b)], to the previously reported oxidative electrochemical protocol [39.8 μg mL(-1) (2a) and 84.2 μg mL(-1) (2b)], for two synthetic cathinones, prevalent on the recreational drugs market. Though not as sensitive as standard HPLC-UV detection, both flow cells show a good agreement, between the quantitative electroanalytical data, thereby making them suitable for the detection and quantification of 4-MMC and 4-MEC, either in their pure form or within complex mixtures. Additionally, the simultaneous HPLC-UV and amperometric detection protocol detailed herein shows a marked improvement and advantage over previously reported electroanalytical methods, which were either unable to selectively discriminate between structurally related synthetic cathinones (e.g. 4-MMC and 4-MEC) or utilised harmful and restrictive materials in their design.
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[Determination of sulpride in human plasma by high performance liquid chromatography].
Yu, X; Luo, Z; Tang, J; Yu, P
1997-11-01
This paper describes a reliable method for the pharmacokinetic study of Sulpride in human plasma by reversed-phase high performance liquid chromatography. To compensate the loss of Sulpride during the extraction procedure we used an internal standard very similar in chemical structure and UV absorbance to those of Sulpride. The mobile phase was methanol-water-acetic acid (60:30:1) with a flow rate of 1.2 mL/min. A UV detector was used at 290 nm. The linear range was 5-100 mg/L and the detectable limit was 1.0 mg/L. The recovery and RSD were 97.95%-99.96% and 2.6%-5.1% respectively. The results showed that this method is a sensitive and accurate one which makes the pharmacokinetic study of Sulpride possible. If the concentration was too low to be detected by UV monitor, a fluorescence detector could be used with the excitation wavelength at 299 nm and emission at 342 nm. We analyzed the plasma samples from 30 day-treated psychotic patients and got the satisfactory results.
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UV-Enhanced Ethanol Sensing Properties of RF Magnetron-Sputtered ZnO Film.
Huang, Jinyu; Du, Yu; Wang, Quan; Zhang, Hao; Geng, Youfu; Li, Xuejin; Tian, Xiaoqing
2017-12-26
ZnO film was deposited by the magnetron sputtering method. The thickness of ZnO film is approximately 2 μm. The influence of UV light illumination on C₂H₅OH sensing properties of ZnO film was investigated. Gas sensing results revealed that the UV-illuminated ZnO film displays excellent C₂H₅OH characteristics in terms of high sensitivity, excellent selectivity, rapid response/recovery, and low detection limit down to 0.1 ppm. The excellent sensing performance of the sensor with UV activation could be attributed to the photocatalytic oxidation of ethanol on the surface of the ZnO film, the planar film structure with high utilizing efficiency of UV light, high electron mobility, and a good surface/volume ratio of of ZnO film with a relatively rough and porous surface.
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Sauveur, C; Baune, A; Vergnes, N; Jeanniot, J P
1989-01-01
A selective and sensitive method for the determination of fenspiride in biological fluids is described. The method involves liquid-liquid extraction followed by separation on a reversed-phase column with electrochemical detection for low levels of the drug in plasma (less than or equal to 100 ng ml-1) or UV absorption for higher concentrations in plasma or urine. The method is suitable for pharmacokinetic analyses and drug monitoring studies.
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Galeotti, Francesco; Barile, Elisa; Lanzotti, Virginia; Dolci, Marcello; Curir, Paolo
2008-01-01
One flavone-C-glycoside and two flavonol-O-glycosides were recognized and isolated as the main flavonoidal components in nine different carnation cultivars, and their chemical structures have been determined by spectroscopic methods, including UV detection, MS and NMR. The distribution of these three compounds in flowers, leaves, stems, young sprouts, and roots of each cultivar was evaluated by a simple HPLC-UV method: the graphic representation of their content in the different tissues allows to identify and characterize unambiguously each considered carnation cultivar. The presented method could be an easy, inexpensive and reliable tool for carnation cultivar discrimination.
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Detection of biological warfare agents using ultra violet-laser induced fluorescence LIDAR
NASA Astrophysics Data System (ADS)
Joshi, Deepti; Kumar, Deepak; Maini, Anil K.; Sharma, Ramesh C.
This review has been written to highlight the threat of biological warfare agents, their types and detection. Bacterial biological agent Bacillus anthracis (bacteria causing the disease anthrax) which is most likely to be employed in biological warfare is being discussed in detail. Standoff detection of biological warfare agents in aerosol form using Ultra violet-Laser Induced Fluorescence (UV-LIF) spectroscopy method has been studied. Range-resolved detection and identification of biological aerosols by both nano-second and non-linear femto-second LIDAR is also discussed. Calculated received fluorescence signal for a cloud of typical biological agent Bacillus globigii (Simulants of B. anthracis) at a location of ˜5.0 km at different concentrations in presence of solar background radiation has been described. Overview of current research efforts in internationally available working UV-LIF LIDAR systems are also mentioned briefly.
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Xu, Yan; Wang, Weilong; Li, Sam Fong Yau
2007-05-01
This report describes a method to simultaneously determine 11 low-molecular-weight (LMW) organic acids and 16 chlorinated acid herbicides within a single run by a portable CE system with contactless conductivity detection (CCD) in a poly(vinyl alcohol) (PVA)-coated capillary. Under the optimized condition, the LODs of CE-CCD ranged from 0.056 to 0.270 ppm, which were better than for indirect UV (IUV) detection of the 11 LMW organic acids or UV detection of the 16 chlorinated acid herbicides. Combined with an on-line field-amplified sample stacking (FASS) procedure, sensitivity enhancement of 632- to 1078-fold was achieved, with satisfactory reproducibility (RSDs of migration times less than 2.2%, and RSDs of peak areas less than 5.1%). The FASS-CE-CCD method was successfully applied to determine the two groups of acidic pollutants in two kinds of environmental water samples. The portable CE-CCD system shows advantages such as simplicity, cost effectiveness, and miniaturization. Therefore, the method presented in this report has great potential for onsite analysis of various pollutants at the trace level.
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Degradation of naproxen by UV, VUV photolysis and their combination.
Arany, Eszter; Szabó, Rita Katalin; Apáti, László; Alapi, Tünde; Ilisz, István; Mazellier, Patrick; Dombi, András; Gajda-Schrantz, Krisztina
2013-11-15
Naproxen is a widely used nonsteroidal anti-inflammatory drug. Recently, this medicine was detected both in natural waters (up to 1.5 μg L(-1)) and in sewage treatment plant effluents (up to 5.2 μg L(-1)). Moreover, naproxen is only partly eliminated by classical processes used in sewage treatment plants. Therefore, its degradation is of utmost interest. Advanced oxidation processes proved to be the most suitable methods for the elimination of persistent organic contaminants. In this work ultraviolet (UV, 254 nm), vacuum ultraviolet photolysis (VUV, 172 nm) and their combination (UV/VUV, 254/185 nm) were investigated. The efficiency of the methods increased in the following order: UV < VUV < UV/VUV photolysis. However, VUV irradiation was found to mineralize the contaminant molecule most effectively. The chemical structures of three out of four aromatic by-products and of some aliphatic carboxylic acids were presumed. The effects of dissolved O2 and the initial concentration of naproxen on the degradation were also investigated. Copyright © 2013 Elsevier B.V. All rights reserved.
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Guo, Hui; Li, Huan; Liu, Xiao; Cai, Hao; Wu, Li; Cai, Bao-Chang
2014-12-01
To develop a high performance liquid chromatography (HPLC) coupled with electrospray ionization mass spectrometry (ESI-MS) and ultraviolet (UV) detector method for the acid-alkaline simultaneous determination of ten bioactive compounds, and analyze the effect of compatible medicinal plants on the concentration of components in Dahuang Fuzi Tang (DFT). The chromatographic separation was performed on a Hypersil BDS C18 analytical column by gradient elution with acetonitrile and formate buffer (containing 0.15% formic acid, V/V) at 25 °C with a flow rate of 1.0 mL·min(-1) and UV detection at 280 nm. Four of the ten compounds in DFT were identified and their MS fragments were elucidated by HPLC-ESI-MS, and the contents of the six compounds were determined by HPLC-UV. All calibration curves showed good linear regression (r(2) ≥ 0.9990). The limits of detection and limits of quantification were 0.021-0.155 -g·mL(-1) and 0.076-0.520 -g·mL(-1), respectively. Overall precision RSD (intra-day and inter-day) were less than 2.96%, and the average recoveries were 98.35%-101.45%, with RSD ranging from 1.54% to 3.01% for the analytes. The developed method can be applied for the quality control and provide analytical evidence on the chemical basis and combinational principles of DFT. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.
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Speciation of inorganic selenium and selenoamino acids by an HPLC-UV-HG-AFS system.
Ipolyi, I; Corns, W; Stockwell, P; Fodor, P
2001-01-01
For the on-line speciation of selenocystine (SeCys), selenomethionine (SeMet), selenoethionine (SeEt), selenite (Se(IV)) and selenate (Se(VI)), a high-performance liquid chromatography-UV irradiation-hydride generation-atomic fluorescence spectro- metric method is described. Separation was carried out on a conventional reversed-phase C18 column modified with didodecyl- dimethylammonium bromide with gradient elution applying two concentrations of ammonium acetate as the mobile phase. UV irradiation and hydride generation parameters were optimized. The obtained detection limits for SeCys, SeMet, SeEt, Se(IV) and Se(VI) were 0.31, 0.43, 0.7, 0.44 and 0.32 ng ml(-1), respectively, using a 100-microl loop. The method was tested with spiked mineral water and two volunteers' urine samples.
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Speciation of inorganic selenium and selenoamino acids by an HPLC-UV-HG-AFS system
Ipolyi, I.; Corns, W.; Stockwell, P.; Fodor, P.
2001-01-01
For the on-line speciation of selenocystine (SeCys), selenomethionine (SeMet), selenoethionine (SeEt), selenite (Se(IV)) and selenate (Se(VI)), a high-performance liquid chromatography-UV irradiation-hydride generation-atomic fluorescence spectro- metric method is described. Separation was carried out on a conventional reversed-phase C18 column modified with didodecyl- dimethylammonium bromide with gradient elution applying two concentrations of ammonium acetate as the mobile phase. UV irradiation and hydride generation parameters were optimized. The obtained detection limits for SeCys, SeMet, SeEt, Se(IV) and Se(VI) were 0.31, 0.43, 0.7, 0.44 and 0.32 ng ml−1, respectively, using a 100-wl loop. The method was tested with spiked mineral water and two volunteers' urine samples. PMID:18924707
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Wang, Lu; Qu, Haibin
2016-03-01
A method combining solid phase extraction, high performance liquid chromatography, and ultraviolet/evaporative light scattering detection (SPE-HPLC-UV/ELSD) was developed according to Quality by Design (QbD) principles and used to assay nine bioactive compounds within a botanical drug, Shenqi Fuzheng Injection. Risk assessment and a Plackett-Burman design were utilized to evaluate the impact of 11 factors on the resolutions and signal-to-noise of chromatographic peaks. Multiple regression and Pareto ranking analysis indicated that the sorbent mass, sample volume, flow rate, column temperature, evaporator temperature, and gas flow rate were statistically significant (p < 0.05) in this procedure. Furthermore, a Box-Behnken design combined with response surface analysis was employed to study the relationships between the quality of SPE-HPLC-UV/ELSD analysis and four significant factors, i.e., flow rate, column temperature, evaporator temperature, and gas flow rate. An analytical design space of SPE-HPLC-UV/ELSD was then constructed by calculated Monte Carlo probability. In the presented approach, the operating parameters of sample preparation, chromatographic separation, and compound detection were investigated simultaneously. Eight terms of method validation, i.e., system-suitability tests, method robustness/ruggedness, sensitivity, precision, repeatability, linearity, accuracy, and stability, were accomplished at a selected working point. These results revealed that the QbD principles were suitable in the development of analytical procedures for samples in complex matrices. Meanwhile, the analytical quality and method robustness were validated by the analytical design space. The presented strategy provides a tutorial on the development of a robust QbD-compliant quantitative method for samples in complex matrices.
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Motta, Erick Vicente da Silva; da Costa, Juliana de Carvalho; Bastos, Jairo Kenupp
2017-09-01
Copaifera langsdorffii Desf. (Fabaceae, Caesalpinioideae), popularly known as "copaiba" or "pau d'óleo", is a species of tree that is found throughout Brazil. The leaves of this tree are used in folk medicine to treat kidney stones. Galloylquinic acid derivatives and flavonoids are the main secondary metabolites found in C. langsdorffii leaves and are likely to be responsible for the effectiveness of this treatment. As an attempt to produce a phytotherapic, we have developed a reliable HPLC-UV method for the quality control of C. langsdorffii leaves. Phenolic compounds were extracted from C. langsdorffii leaves using 70% aqueous ethanol as the extraction solvent. HPLC-UV analyses were carried out on a Synergi Polar-RP column (100×3.0mm, 2.5μm), and the mobile phase was made up of formic acid-water (0.1:99.9, solvent A), and isopropanol-methanol-acetonitrile (5:40:60, solvent B). The elution gradient was A:B (90:10 to 85:15) in 8.0min, followed by A:B (85:15 to 64:36) up to 30.0min, using a flow rate of 0.7mL/min, and UV detection at 280nm. This method was used to quantify nine galloylquinic acid derivatives and two flavonoids, which gave a good detection response and linearity in the range of 1.88-110.0μg/mL. Furthermore, the detection and quantification limits ranged from 0.070 to 0.752μg/mL, and 0.211-2.278μg/mL respectively, with a maximum RSD of 4.18%. The method is reliable for the quality control of C. langsdorffii raw material, its hydroethanolic extract, and could potentially be used to quantify these compounds in other Copaifera species. Copyright © 2017 Elsevier B.V. All rights reserved.
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Zhang, Ying; Li, Yan; Zhu, Xiao-Juan; Li, Min; Chen, Hao-Yu; Lv, Xiao-Ling; Zhang, Jian
2017-07-01
A reliable and accurate method for the determination of seven biogenic amines (BAs) was developed and validated with Chinese rice wine samples. The BAs were derivatised with dansyl chloride, cleaned up using solid-phase extraction (SPE) and separated by high-performance liquid chromatography (HPLC) coupled with ultraviolet (UV) detection. The optimised derivatisation reaction, conducted at pH 9.6 and 60°C for 30 min, ensured baseline separation and peak symmetry for each BA. SPE clean-up using Oasis MCX cartridges yielded good recovery rates for all BAs and effectively reduced matrix effects. The developed method shows good linearity with determination coefficients of more than 0.9989 over a concentration range of 0.1-100 mg l -1 . The limits of detection (LODs) for the investigated BAs ranged from 2.07 to 5.56 µg l -1 . The intra- and inter-day relative standard deviations (RSDs) ranged from 0.86% to 3.81% and from 2.13% to 3.82%, respectively. Spiking experiments showed that the overall recovery rates ranged from 85% to 113%. Thus, the proposed method was demonstrated as being suitable for simultaneous detection, with accurate and precise quantification, of BAs in Chinese rice wine.
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Low-level luminescence as a method of detecting the UV influence on biological systems
NASA Astrophysics Data System (ADS)
Mei, Wei-Ping; Popp, Fritz A.
1995-02-01
It is well known that low-level luminescence is correlated to many physiological and biological parameters, e.g. cell cycle, temperature, oxidation- and UV-stress. We report some new approaches on low-level luminescence measurements and UV influence on different biological systems. One example concerns yeast cultures, which show an increasing intensity of luminescence after UV-treatment with a maximum after 1.5 h. Investigations on normal human fibroblasts and keratinocytes display different longtime kinetics: The former show no changes of the luminescence in time, the latter an increase that reaches the maximum after 9 h. The time-dependent spectral measurement on xeroderma pigmentosum after UV-treatment displays a time-shift of the action-spectra shifting the maximum from 400 nm to 420 nm in 12 h. Some results on neutrophils reveals spectral UV influence on respiratory burst and the cellular repair system. The results on human skin display spectral changes of low-level luminescence after UV-treatment. These results provide a useful tool of analyzing UV influence on human skin.
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Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad
2016-01-01
The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 µg/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3) for chloramphenicol (12.5 µg/Kg) and florfenicol (12.2 µg/Kg), and precision with relative standard deviation values under 15% (RSD, n = 3). Good recoveries (69.1-79.4%) were obtained for the extraction of the target analytes in milk samples. This simple and economic method has been applied for analyses of 15 real milk samples. Among all samples only one of them was contaminated to florfenicol; 62.4 µg/Kg and contamination to chloramphenicol was not detected.
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Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad
2016-01-01
The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 µg/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3) for chloramphenicol (12.5 µg/Kg) and florfenicol (12.2 µg/Kg), and precision with relative standard deviation values under 15% (RSD, n = 3). Good recoveries (69.1–79.4%) were obtained for the extraction of the target analytes in milk samples. This simple and economic method has been applied for analyses of 15 real milk samples. Among all samples only one of them was contaminated to florfenicol; 62.4 µg/Kg and contamination to chloramphenicol was not detected. PMID:27980571
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Cap, Andrew P.; Pidcoke, Heather F.; Keil, Shawn D.; Staples, Hilary M.; Anantpadma, Manu; Carrion, Ricardo; Davey, Robert A.; Frazer-Abel, Ashley; Taylor, Audra L.; Gonzales, Richard; Patterson, Jean L.; Goodrich, Raymond P.
2018-01-01
BACKGROUND Transfusion of plasma from recovered patients after Ebolavirus (EBOV) infection, typically called ‘convalescent plasma,’ is an effective treatment for active disease available in endemic areas, but carries the risk of introducing other pathogens, including other strains of EBOV. A pathogen reduction technology using ultraviolet light and riboflavin (UV + RB) is effective against multiple enveloped, negative-sense, single-stranded RNA viruses that are similar in structure to EBOV. We hypothesized that UV + RB is effective against EBOV in blood products without activating complement or reducing protective immunoglobulin titers that are important for the treatment of ebolavirus disease (EVD). STUDY DESIGN AND METHODS Four in vitro experiments were conducted to evaluate effects of UV + RB on green fluorescent protein EBOV (EBOV-GFP), wild-type EBOV in serum and whole blood, respectively, and on immunoglobulins and complement in plasma. Initial titers for Experiments 1–3 were: 4.21 log10 GFP units/mL, 4.96 log10 infectious units per mL, and 4.23 log10 plaque forming units per mL (PFU/mL). Conditions tested in the first three experiments included: 1. EBOV-GFP + UV + RB; 2. EBOV-GFP + RB only; 3 EBOV-GFP + UV only; 4. EBOV-GFP without RB or UV; 5. Virus-free control + UV only; and 6. Virus-free control without RB or UV. RESULTS UV + RB reduced EBOV titers to non-detectable levels in both non-human primate serum (≥ 2.8 to 3.2 log reduction) and human whole blood (≥ 3.0 log reduction) without decreasing protective antibody titers in human plasma. CONCLUSION Our in vitro results demonstrate that the UV + RB treatment efficiently reduces EBOV titers to below limits of detection in both serum and whole blood. In vivo testing to determine whether UV + RB can improve convalescent blood product safety is indicated. PMID:27001363
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Surdu, Simona; Fitzgerald, Edward F.; Bloom, Michael S.; Boscoe, Francis P.; Carpenter, David O.; Haase, Richard F.; Gurzau, Eugen; Rudnai, Peter; Koppova, Kvetoslava; Févotte, Joëlle; Leonardi, Giovanni; Vahter, Marie; Goessler, Walter; Kumar, Rajiv; Fletcher, Tony
2013-01-01
Background Studies suggest that ambient sunlight plays an important role in the pathogenesis of non-melanoma skin cancers (NMSC). However, there is ongoing controversy regarding the relevance of occupational exposure to natural and artificial ultraviolet radiation (UV) radiation. Objectives We investigated potential associations between natural and artificial UV radiation exposure at work with NMSC in a case-control study conducted in Hungary, Romania, and Slovakia. Methods Occupational exposures were classified by expert assessment for 527 controls and 618 NMSC cases (515 basal cell carcinoma, BCC). Covariate information was collected via interview and multiple logistic regression models were used to assess associations between UV exposure and NMSC. Results Lifetime prevalence of occupational exposure in the participants was 13% for natural UV radiation and 7% for artificial UV radiation. Significant negative associations between occupational exposure to natural UV radiation and NMSC were detected for all who had ever been exposed (odds ratio (OR) 0.47, 95% confidence interval (CI) 0.27–0.80); similar results were detected using a semi-quantitative metric of cumulative exposure. The effects were modified by skin complexion, with significantly decreased risks of BCC among participants with light skin complexion. No associations were observed in relation to occupational artificial UV radiation exposure. Conclusions The protective effect of occupational exposure to natural UV radiation was unexpected, but limited to light-skinned people, suggesting adequate sun-protection behaviors. Further investigations focusing on variations in the individual genetic susceptibility and potential interactions with environmental and other relevant factors are planned. PMID:23638051
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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.
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UV Spectrophotometric Method for Estimation of Polypeptide-K in Bulk and Tablet Dosage Forms
NASA Astrophysics Data System (ADS)
Kaur, P.; Singh, S. Kumar; Gulati, M.; Vaidya, Y.
2016-01-01
An analytical method for estimation of polypeptide-k using UV spectrophotometry has been developed and validated for bulk as well as tablet dosage form. The developed method was validated for linearity, precision, accuracy, specificity, robustness, detection, and quantitation limits. The method has shown good linearity over the range from 100.0 to 300.0 μg/ml with a correlation coefficient of 0.9943. The percentage recovery of 99.88% showed that the method was highly accurate. The precision demonstrated relative standard deviation of less than 2.0%. The LOD and LOQ of the method were found to be 4.4 and 13.33, respectively. The study established that the proposed method is reliable, specific, reproducible, and cost-effective for the determination of polypeptide-k.
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An automated method for the determination of carbendazim in water that combines high-performance immunoaffinity chromatography (HPIAC), high-performance liquid chromatography (HPLC) in the reversed-phase mode, and detection by either UV-Vis diode array detector (DAD) spectroscopy...
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Ford, Michael J; Deibel, Michael A.; Tomkins, Bruce A
Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methodsmore » determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.« less
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Khairy, Mostafa A; Mansour, Fotouh R
2017-01-01
A reversed-phase HPLC method was developed for the simultaneous determination of ursodeoxycholic acid (UDCA) and the epimeric isomer, chenodeoxycholic acid (CDCA), in their synthetic mixtures and in tablet dosage form. The proposed HPLC method uses a C18 column and mobile phase consisting of an acetonitrile-phosphate buffer mixture (pH 2.3, 100 mM; 50 + 50, v/v) at a flow rate of 2.0 mL/min with UV detection at 210 nm. The method was validated according to the International Conference on Harmonization guidelines; and linearity, range, accuracy, precision, robustness, and system suitability were studied. The LOD and LOQ were also calculated and found to be 1.23 and 3.73 μg/mL for UDCA and 0.83 and 2.52 μg/mL for CDCA, respectively. The method was adapted for UHPLC, in which baseline separation was achieved in <2.5 min. The assay results of Ursomix tablets by the developed method were statistically compared with those obtained by the reference method using t- and F-tests, and no significant differences were observed.
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Pires, Adriana Elias; Honda, Neli Kiko; Cardoso, Cláudia Andréa Lima
2004-10-29
A method for sample preparation and analysis by high performance liquid chromatography with UV detection (HPLC-UV) has been developed for routine analysis of psoralen and bergapten, photosensitizing compounds, in oral solutions of phytomedicines employed in Brazil for some illnesses. The linearity, accuracy, the inter- and intra-day precision of the procedure were evaluated. Calibration curves for psoralen and bergapten were linear in the range of 1.0-600.0 microg ml(-1) and 1.0-400.0 microg ml(-1) respectively. The recoveries of the psoralens in the oral solutions analysed were 94.43-99.97%. The percentage coefficient of variation (CV) of the quantitative analysis of the psoralens in the products analysis was within 5%. In inter-equipment study was employed gas chromatography-flame ionization (CG-FID) detection.
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Zinellu, Angelo; Sotgia, Salvatore; Zinellu, Elisabetta; Chessa, Roberto; Deiana, Luca; Carru, Ciriaco
2006-03-01
Guanidinoacetic acid (GAA) measurement has recently become of great interest for the diagnosis of creatine (Cn) metabolism disorders, and research calls for rapid and inexpensive methods for its detection in plasma and urine in order to assess a large number of patients. We propose a new assay for the measurement of GAA by a simple CZE UV-detection without previous sample derivatization. Plasma samples were filtered by Microcon-10 microconcentrators and directly injected into the capillary, while for urine specimens a simple water dilution before injection was needed. A baseline separation was obtained in less than 8 min using a 60.2 cm x 75 microm uncoated silica capillary, 75 mmol/L Tris-phosphate buffer pH 2.25 at 15 degrees C. The performance of the developed method was assessed by measuring plasma creatinine and Cn in 32 normal subjects and comparing the data obtained by the new method with those found with the previous CE assay. Our new method seems to be an inexpensive, fast and specific tool to assess a large number of patients both in clinical and in research laboratories.
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NASA Astrophysics Data System (ADS)
Bhartia, R.; Wanger, G.; Orphan, V. J.; Fries, M.; Rowe, A. R.; Nealson, K. H.; Abbey, W. J.; DeFlores, L. P.; Beegle, L. W.
2014-12-01
Detection of in situ biosignatures on terrestrial and planetary missions is becoming increasingly more important. Missions that target the Earth's deep biosphere, Mars, moons of Jupiter (including Europa), moons of Saturn (Titan and Enceladus), and small bodies such as asteroids or comets require methods that enable detection of materials for both in-situ analysis that preserve context and as a means to select high priority sample for return to Earth. In situ instrumentation for biosignature detection spans a wide range of analytical and spectroscopic methods that capitalize on amino acid distribution, chirality, lipid composition, isotopic fractionation, or textures that persist in the environment. Many of the existing analytical instruments are bulk analysis methods and while highly sensitive, these require sample acquisition and sample processing. However, by combining with triaging spectroscopic methods, biosignatures can be targeted on a surface and preserve spatial context (including mineralogy, textures, and organic distribution). To provide spatially correlated chemical analysis at multiple spatial scales (meters to microns) we have employed a dual spectroscopic approach that capitalizes on high sensitivity deep UV native fluorescence detection and high specificity deep UV Raman analysis.. Recently selected as a payload on the Mars 2020 mission, SHERLOC incorporates these optical methods for potential biosignatures detection on Mars. We present data from both Earth analogs that operate as our only examples known biosignatures and meteorite samples that provide an example of abiotic organic formation, and demonstrate how provenance effects the spatial distribution and composition of organics.
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Varden, Lara; Smith, Britannia; Bou-Abdallah, Fadi
2017-01-01
Capillary zone electrophoresis (CZE) is a sensitive and rapid technique used for determining traces of inorganic and organic anions in potable, natural, and wastewaters. Here, CZE with indirect UV-diode array detection (CZE-DAD) was employed with a background electrolyte system comprising of an Agilent Technologies proprietary basic anion buffer at pH 12.0 and a forensic anion detection method. The limits of detection (LOD) for this method ranged between 3 and 5 ppm and involved hydrodynamic injection of 50 mbar for 6 s with a negative polarity separation voltage of −30 kV at 30°C, a detection wavelength of 350 nm and indirect reference of 275 nm. Fourteen different anions were checked for in the water samples that were examined and included bromide, chloride, thiosulfate, nitrate, nitrite, sulfate, azide, carbonate, fluoride, arsenate, phosphate, acetate, lactate, and silicate. The water samples were collected from Northern New York towns and the Raquette River water system, the third longest river in New York State and the largest watershed of the central and western Adirondacks. The concentrations detected for these anions ranged from <5.0 ppm to 260 ppm. PMID:29057145
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Wang, George; Tomasella, Frank P
2016-06-01
Ion-pairing high-performance liquid chromatography-ultraviolet (HPLC-UV) methods were developed to determine two commonly used chelating agents, ethylenediaminetetraacetic acid (EDTA) in Abilify® (a small molecule drug with aripiprazole as the active pharmaceutical ingredient) oral solution and diethylenetriaminepentaacetic acid (DTPA) in Yervoy® (a monoclonal antibody drug with ipilimumab as the active pharmaceutical ingredient) intravenous formulation. Since the analytes, EDTA and DTPA, do not contain chromophores, transition metal ions (Cu 2+ , Fe 3+ ) which generate highly stable metallocomplexes with the chelating agents were added into the sample preparation to enhance UV detection. The use of metallocomplexes with ion-pairing chromatography provides the ability to achieve the desired sensitivity and selectivity in the development of the method. Specifically, the sample preparation involving metallocomplex formation allowed sensitive UV detection. Copper was utilized for the determination of EDTA and iron was utilized for the determination of DTPA. In the case of EDTA, a gradient mobile phase separated the components of the formulation from the analyte. In the method for DTPA, the active drug substance, ipilimumab, was eluted in the void. In addition, the optimization of the concentration of the ion-pairing reagent was discussed as a means of enhancing the retention of the aminopolycarboxylic acids (APCAs) including EDTA and DTPA and the specificity of the method. The analytical method development was designed based on the chromatographic properties of the analytes, the nature of the sample matrix and the intended purpose of the method. Validation data were presented for the two methods. Finally, both methods were successfully utilized in determining the fate of the chelates.
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NASA Astrophysics Data System (ADS)
Chwirot, B. W.; Chwirot, S.; Jedrzejczyk, W.; Redzinski, J.; Raczynska, A. M.; Telega, K.
2001-07-01
We studied spectral and spatial distributions of the intensity of the ultraviolet light-excited fluorescence of human skin. Our studied performed in situ in 162 patients with malignant and non-malignant skin lesions resulted in a new method of detecting melanomas in situ using digital imaging of the spectrally resolved fluorescence. With our diagnostic algorithm we could successfully detect 88.5% of the cases of melanoma in the group of patients subject to examinations with the fluorescence method. A patent application for the method has been submitted to the Patent Office in Warsaw.
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High-performance optical projection controllable ZnO nanorod arrays for microweighing sensors.
Wang, Hongbo; Jiang, Shulan; Zhang, Lei; Yu, Bingjun; Chen, Duoli; Yang, Weiqing; Qian, Linmao
2018-03-08
Optical microweighing sensors are an essential component of micro-force measurements in physical, chemical, and biological detection fields, although, their limited detection range (less than 15°) severely hinders their wide application. Such a limitation is mainly attributed to the essential restrictions of traditional light reflection and optical waveguide modes. Here, we report a high-performance optical microweighing sensor based on the synergistic effects of both a new optical projection mode and a ZnO nanorod array sensor. Ascribed to the unique configuration design of this sensing method, this optical microweighing sensor has a wide detection range (more than 80°) and a high sensitivity of 90 nA deg -1 , which is much larger than that of conventional microcantilever-based optical microweighing sensors. Furthermore, the location of the UV light source can be adjusted within a few millimeters, meaning that the microweighing sensor does not need repetitive optical calibration. More importantly, for low height and small incident angles of the UV light source, we can obtain highly sensitive microweighing properties on account of the highly sensitive ZnO nanorod array-based UV sensor. Therefore, this kind of large detection range, non-contact, and non-destructive microweighing sensor has potential applications in air quality monitoring and chemical and biological detection.
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Study of UV imaging technology for noninvasive detection of latent fingerprints
NASA Astrophysics Data System (ADS)
Li, Hong-xia; Cao, Jing; Niu, Jie-qing; Huang, Yun-gang
2013-09-01
Using UV imaging technology, according to the special absorption 、reflection 、scattering and fluorescence characterization of the various residues in fingerprints (fatty acid ester, protein, and carboxylic acid salts etc) to the UV light, weaken or eliminate the background disturbance to increase the brightness contrast of fingerprints with the background, and design、setup the illumination optical system and UV imaging system, the noninvasive detection of latent fingerprints remaining on various object surface are studied. In the illumination optical system, using the 266nm UV Nd:YAG solid state laser as illumination light source, by calculating the best coupling conditions of the laser beam with UV liquid core fiber and analyzing the beam transforming characterizations, we designed and setup the optical system to realize the UV imaging uniform illumination. In the UV imaging system, the UV lens is selected as the fingerprint imaging element, and the UV intensified CCD (ICCD) which consists of a second-generation UV image intensifier and a CCD coupled by fiber plate and taper directly are used as the imaging sensing element. The best imaging conditions of the UV lens with ICCD were analyzed and the imaging system was designed and setup. In this study, by analyzing the factors which influence the detection effect, optimal design and setup the illumination system and imaging system, latent fingerprints on the surface of the paint tin box、plastic、smooth paper、notebook paper and print paper were noninvasive detected and appeared, and the result meet the fingerprint identification requirements in forensic science.
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Hoffman, Justin T; Rossi, Steven S; Espina-Quinto, Rowena; Letendre, Scott; Capparelli, Edmund V
2013-01-01
Background Previously published methods for determination of efavirenz (EFV) in human dried blood spots (DBS) employ costly and complex liquid chromatography/mass spectrometry. We describe the validation and evaluation of a simple and inexpensive high-performance liquid chromatography (HPLC) method for EFV quantification in human DBS and dried plasma spots (DPS), using ultraviolet (UV) detection appropriate for resource-limited settings. Methods 100μl of heparinized whole blood or plasma were spotted onto blood collection cards, dried, punched, and eluted. Eluates are injected onto a C-18 reversed phase HPLC column. EFV is separated isocratically using a potassium phosphate and ACN mobile phase. UV detection is at 245nm. Quantitation is by use of external calibration standards. Following validation, the method was evaluated using whole blood and plasma from HIV-positive patients undergoing EFV therapy. Results Mean recovery of drug from dried blood spots is 91.5%. The method is linear over the validated concentration range of 0.3125 – 20.0μg/mL. A good correlation (Spearman r=0.96) between paired plasma and DBS EFV concentrations from the clinical samples was observed, and hematocrit level was not found to be a significant determinant of the EFV DBS level. The mean observed CDBS/Cplasma ratio was 0.68. A good correlation (Spearman r=0.96) between paired plasma and DPS EFV concentrations from the clinical samples was observed. The mean percent deviation of DPS samples from plasma samples is 1.68%. Conclusions Dried whole blood spot or dried plasma spot sampling is well suited for monitoring EFV therapy in resource limited settings, particularly when high sensitivity is not essential. PMID:23503446
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Kallio, Heikki; Yang, Wei; Liu, Pengzhan; Yang, Baoru
2014-08-06
A rapid and sensitive method for profiling of proanthocyanidins (PAs) of sea buckthorn (Hippophaë rhamnoides) berries was established based on aqueous, acidified acetone extraction. The extract was purified by Sephadex column chromatography and analyzed using reversed-phase, normal-phase, and hydrophilic interaction liquid chromatography (HILIC). Negative ion electrospray ionization mass spectrometry (ESI-MS) in single ion recording (SIR) and full scan modes combined with UV detection were used to define the combinations and ratios of PA oligomer classes. PAs with degree of polymerization from 2 to 11 were detected by HILIC-ESI-MS. Quantification of dimeric, trimeric, and tetrameric PAs was carried out with ESI-MS-SIR, and their molar proportions were 40, 40, and 20%, respectively. Only B-type PAs were found, and (epi)gallocatechins were the main monomeric units. More than 60 combinations of (epi)catechins and (epi)gallocatechins of proanthocyanidin dimers and trimers were found. A majority of the PAs were shown to be higher polymers based on the HILIC-UV analysis.
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Yeh, Li-Ko; Luo, Jie-Chun; Chen, Min-Chun; Wu, Chih-Hung; Chen, Jian-Zhang; Cheng, I-Chun; Hsu, Cheng-Che; Tian, Wei-Cheng
2016-01-01
A photoactivated gas detector operated at room temperature was microfabricated using a simple hydrothermal method. We report that the photoactivated gas detector can detect toluene using a UV illumination of 2 μW/cm2. By ultraviolet (UV) illumination, gas detectors sense toluene at room temperature without heating. A significant enhancement of detector sensitivity is achieved because of the high surface-area-to-volume ratio of the morphology of the coral-like ZnO nanorods arrays (NRAs) and the increased number of photo-induced oxygen ions under UV illumination. The corresponding sensitivity (ΔR/R0) of the detector based on coral-like ZnO NRAs is enhanced by approximately 1022% compared to that of thin-film detectors. The proposed detector greatly extends the dynamic range of detection of metal-oxide-based detectors for gas sensing applications. We report the first-ever detection of toluene with a novel coral-like NRAs gas detector at room temperature. A sensing mechanism model is also proposed to explain the sensing responses of gas detectors based on coral-like ZnO NRAs. PMID:27809222
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Yeh, Li-Ko; Luo, Jie-Chun; Chen, Min-Chun; Wu, Chih-Hung; Chen, Jian-Zhang; Cheng, I-Chun; Hsu, Cheng-Che; Tian, Wei-Cheng
2016-10-31
A photoactivated gas detector operated at room temperature was microfabricated using a simple hydrothermal method. We report that the photoactivated gas detector can detect toluene using a UV illumination of 2 μW/cm². By ultraviolet (UV) illumination, gas detectors sense toluene at room temperature without heating. A significant enhancement of detector sensitivity is achieved because of the high surface-area-to-volume ratio of the morphology of the coral-like ZnO nanorods arrays (NRAs) and the increased number of photo-induced oxygen ions under UV illumination. The corresponding sensitivity (ΔR/R₀) of the detector based on coral-like ZnO NRAs is enhanced by approximately 1022% compared to that of thin-film detectors. The proposed detector greatly extends the dynamic range of detection of metal-oxide-based detectors for gas sensing applications. We report the first-ever detection of toluene with a novel coral-like NRAs gas detector at room temperature. A sensing mechanism model is also proposed to explain the sensing responses of gas detectors based on coral-like ZnO NRAs.
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Mendez, Andreas S L; Steppe, Martin; Schapoval, Elfrides E S
2003-12-04
A high-performance liquid chromatographic method and a UV spectrophotometric method for the quantitative determination of meropenem, a highly active carbapenem antibiotic, in powder for injection were developed in present work. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by reversed-phase technique on an RP-18 column with a mobile phase composed of 30 mM monobasic phosphate buffer and acetonitrile (90:10; v/v), adjusted to pH 3.0 with orthophosphoric acid. The UV spectrophotometric method was performed at 298 nm. The samples were prepared in water and the stability of meropenem in aqueous solution at 4 and 25 degrees C was studied. The results were satisfactory with good stability after 24 h at 4 degrees C. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and can be used for the reliable quantitation of meropenem in pharmaceutical dosage form.
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Determination of hydroxyurea in human plasma by HPLC-UV using derivatization with xanthydrol.
Legrand, Tiphaine; Rakotoson, Marie-Georgine; Galactéros, Frédéric; Bartolucci, Pablo; Hulin, Anne
2017-10-01
A simple and rapid high performance liquid chromatography (HPLC) method using ultraviolet (UV) detection was developed to determine hydroxyurea (HU) concentration in plasma sample after derivatization with xanthydrol. Two hundred microliters samples were spiked with methylurea (MeU) as internal standard and proteins were precipitated by adding methanol. Derivatization of HU and MeU was immediately performed by adding 0.02M xanthydrol and 1.5M HCl in order to obtain xanthyl-derivatives of HU and MeU that can be further separated using HPLC and quantified using UV detection at 240nm. Separation was achieved using a C18 column with a mobile phase composed of 20mM ammonium acetate and acetonitrile in gradient elution mode at a flow rate of 1mL/min. The total analysis time did not exceed 18min. The method was found linear from 5 to 400μM and all validation parameters fulfilled the international requirements. Between- and within-run accuracy error ranged from -4.7% to 3.2% and precision was lower than 12.8%. This simple method requires small volume samples and can be easily implemented in most clinical laboratories to develop pharmacokinetics studies of HU and to promote its therapeutic monitoring. Copyright © 2017 Elsevier B.V. All rights reserved.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Thornton, Michelle
Capillary electrophoresis (CE) is an effective method for separating ionic species according to differences in their electrophoretic mobilities. CE separations of amino acids by direct detection are difficult due to their similar electrophoretic mobilities and low absorbances. However, native amino acids can be separated by CE as cations at a low pH by adding an alkanesulfonic acid to the electrolyte carrier which imparts selectivity to the system. Derivatization is unnecessary when direct UV detection is used at 185 nm. Simultaneous speciation of metal cations such as vanadium (IV) and vanadium (V) can easily be performed without complexation prior to analysis.more » An indirect UV detection scheme for acidic conditions was also developed using guanidine as the background carrier electrolyte (BCE) for the indirect detection of metal cations. Three chapters have been removed for separate processing. This report contains introductory material, references, and general conclusions. 80 refs.« less
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Detection of biological warfare agents using ultra violet-laser induced fluorescence LIDAR.
Joshi, Deepti; Kumar, Deepak; Maini, Anil K; Sharma, Ramesh C
2013-08-01
This review has been written to highlight the threat of biological warfare agents, their types and detection. Bacterial biological agent Bacillus anthracis (bacteria causing the disease anthrax) which is most likely to be employed in biological warfare is being discussed in detail. Standoff detection of biological warfare agents in aerosol form using Ultra violet-Laser Induced Fluorescence (UV-LIF) spectroscopy method has been studied. Range-resolved detection and identification of biological aerosols by both nano-second and non-linear femto-second LIDAR is also discussed. Calculated received fluorescence signal for a cloud of typical biological agent Bacillus globigii (Simulants of B. anthracis) at a location of ~5.0 km at different concentrations in presence of solar background radiation has been described. Overview of current research efforts in internationally available working UV-LIF LIDAR systems are also mentioned briefly. Copyright © 2013 Elsevier B.V. All rights reserved.
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Joki-Erkkilä, Minna; Rainio, Juha; Huhtala, Heini; Salonen, Aki; Karhunen, Pekka J
2014-09-01
New clinical forensic examination techniques for sexual assaults have not been introduced over the last few decades. We evaluated the benefit of ultraviolet light compared to white light for detecting minor anogenital injuries and scars, following consensual sexual intercourse among adult volunteers. A prospective study comparing female genital findings utilising white and ultraviolet light. A colposcopy with photographic documentation was used. Personal invitation to healthcare students, hospital employees or acquaintances to volunteer for a gynecological examination, with a focus on clinical forensic aspects. Eighty-eight adult female volunteers were recruited for the study. The examination was performed after consensual intercourse. Age ranged from 20 to 52 years (median 26.5 years). Presence of acute findings and scars in the genital area using white and UV-light. Acute genital injury rate was 14.8% under white light colposcopy and 23.0% using UV light. Submucosal hemorrhages in the genital area were documented significantly better under UV-light than white light (14.9% vs. 6.8%; p=0.016), whereas petechiaes (4.5%) and abrasions (2.3%) were detected using either method. UV-light revealed significantly more often delivery-associated genital scars compared to white light (39.8% vs. 31.8%; p=0.016). Furthermore, 10 out of 31 (33.3%) women had no residual anogenital skin or mucosal surface findings, despite a prior episiotomy or rupture of the vaginal outlet wall during delivery, supporting its enormous ability to heal even after major trauma. UV-light may provide additional value for the evaluation of physical findings in clinical forensic examinations after sexual assault, and is especially useful in detecting otherwise invisible early submucosal hemorrhages and scars. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.
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Deep Galex Observations of the Coma Cluster: Source Catalog and Galaxy Counts
NASA Technical Reports Server (NTRS)
Hammer, D.; Hornschemeier, A. E.; Mobasher, B.; Miller, N.; Smith, R.; Arnouts, S.; Milliard, B.; Jenkins, L.
2010-01-01
We present a source catalog from deep 26 ks GALEX observations of the Coma cluster in the far-UV (FUV; 1530 Angstroms) and near-UV (NUV; 2310 Angstroms) wavebands. The observed field is centered 0.9 deg. (1.6 Mpc) south-west of the Coma core, and has full optical photometric coverage by SDSS and spectroscopic coverage to r-21. The catalog consists of 9700 galaxies with GALEX and SDSS photometry, including 242 spectroscopically-confirmed Coma member galaxies that range from giant spirals and elliptical galaxies to dwarf irregular and early-type galaxies. The full multi-wavelength catalog (cluster plus background galaxies) is 80% complete to NUV=23 and FUV=23.5, and has a limiting depth at NUV=24.5 and FUV=25.0 which corresponds to a star formation rate of 10(exp -3) solar mass yr(sup -1) at the distance of Coma. The GALEX images presented here are very deep and include detections of many resolved cluster members superposed on a dense field of unresolved background galaxies. This required a two-fold approach to generating a source catalog: we used a Bayesian deblending algorithm to measure faint and compact sources (using SDSS coordinates as a position prior), and used the GALEX pipeline catalog for bright and/or extended objects. We performed simulations to assess the importance of systematic effects (e.g. object blends, source confusion, Eddington Bias) that influence source detection and photometry when using both methods. The Bayesian deblending method roughly doubles the number of source detections and provides reliable photometry to a few magnitudes deeper than the GALEX pipeline catalog. This method is also free from source confusion over the UV magnitude range studied here: conversely, we estimate that the GALEX pipeline catalogs are confusion limited at NUV approximately 23 and FUV approximately 24. We have measured the total UV galaxy counts using our catalog and report a 50% excess of counts across FUV=22-23.5 and NUV=21.5-23 relative to previous GALEX measurements, which is not attributed to cluster member galaxies. Our galaxy counts are a better match to deeper UV counts measured with HST.
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Nissen, Mona; Doherty, Brenda; Hamperl, Jonas; Kobelke, Jens; Weber, Karina; Henkel, Thomas; Schmidt, Markus A
2018-02-06
Due to a worldwide increased use of pharmaceuticals and, in particular, antibiotics, a growing number of these substance residues now contaminate natural water resources and drinking supplies. This triggers a considerable demand for low-cost, high-sensitivity methods for monitoring water quality. Since many biological substances exhibit strong and characteristic absorption features at wavelengths shorter than 300 nm, UV spectroscopy presents a suitable approach for the quantitative identification of such water-contaminating species. However, current UV spectroscopic devices often show limited light-matter interaction lengths, demand sophisticated and bulky experimental infrastructure which is not compatible with microfluidics, and leave large fractions of the sample analyte unused. Here, we introduce the concept of UV spectroscopy in liquid-filled anti-resonant hollow core fibers, with large core diameters and lengths of approximately 1 m, as a means to overcome such limitations. This extended light-matter interaction length principally improves the concentration detection limit by two orders of magnitude while using almost the entire sample volume-that is three orders of magnitude smaller compared to cuvette based approaches. By integrating the fibers into an optofluidic chip environment and operating within the lowest experimentally feasible transmission band, concentrations of the application-relevant pharmaceutical substances, sulfamethoxazole (SMX) and sodium salicylate (SS), were detectable down to 0.1 µM (26 ppb) and 0.4 µM (64 ppb), respectively, with the potential to reach significantly lower detection limits for further device integration.
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Nissen, Mona; Doherty, Brenda; Hamperl, Jonas; Kobelke, Jens; Weber, Karina; Henkel, Thomas; Schmidt, Markus A.
2018-01-01
Due to a worldwide increased use of pharmaceuticals and, in particular, antibiotics, a growing number of these substance residues now contaminate natural water resources and drinking supplies. This triggers a considerable demand for low-cost, high-sensitivity methods for monitoring water quality. Since many biological substances exhibit strong and characteristic absorption features at wavelengths shorter than 300 nm, UV spectroscopy presents a suitable approach for the quantitative identification of such water-contaminating species. However, current UV spectroscopic devices often show limited light-matter interaction lengths, demand sophisticated and bulky experimental infrastructure which is not compatible with microfluidics, and leave large fractions of the sample analyte unused. Here, we introduce the concept of UV spectroscopy in liquid-filled anti-resonant hollow core fibers, with large core diameters and lengths of approximately 1 m, as a means to overcome such limitations. This extended light-matter interaction length principally improves the concentration detection limit by two orders of magnitude while using almost the entire sample volume—that is three orders of magnitude smaller compared to cuvette based approaches. By integrating the fibers into an optofluidic chip environment and operating within the lowest experimentally feasible transmission band, concentrations of the application-relevant pharmaceutical substances, sulfamethoxazole (SMX) and sodium salicylate (SS), were detectable down to 0.1 µM (26 ppb) and 0.4 µM (64 ppb), respectively, with the potential to reach significantly lower detection limits for further device integration. PMID:29415468
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Fabrication of antibody microarrays by light-induced covalent and oriented immobilization.
Adak, Avijit K; Li, Ben-Yuan; Huang, Li-De; Lin, Ting-Wei; Chang, Tsung-Che; Hwang, Kuo Chu; Lin, Chun-Cheng
2014-07-09
Antibody microarrays have important applications for the sensitive detection of biologically important target molecules and as biosensors for clinical applications. Microarrays produced by oriented immobilization of antibodies generally have higher antigen-binding capacities than those in which antibodies are immobilized with random orientations. Here, we present a UV photo-cross-linking approach that utilizes boronic acid to achieve oriented immobilization of an antibody on a surface while retaining the antigen-binding activity of the immobilized antibody. A photoactive boronic acid probe was designed and synthesized in which boronic acid provided good affinity and specificity for the recognition of glycan chains on the Fc region of the antibody, enabling covalent tethering to the antibody upon exposure to UV light. Once irradiated with optimal UV exposure (16 mW/cm(2)), significant antibody immobilization on a boronic acid-presenting surface with maximal antigen detection sensitivity in a single step was achieved, thus obviating the necessity of prior antibody modifications. The developed approach is highly modular, as demonstrated by its implementation in sensitive sandwich immunoassays for the protein analytes Ricinus communis agglutinin 120, human prostate-specific antigen, and interleukin-6 with limits of detection of 7.4, 29, and 16 pM, respectively. Furthermore, the present system enabled the detection of multiple analytes in samples without any noticeable cross-reactivities. Antibody coupling via the use of boronic acid and UV light represents a practical, oriented immobilization method with significant implications for the construction of a large array of immunosensors for diagnostic applications.
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Wankhede, S. B.; Raka, K. C.; Wadkar, S. B.; Chitlange, S. S.
2010-01-01
Two UV-spectrophotometric and one reverse phase high performance liquid chromatography methods have been developed for the simultaneous estimation of amlodipine besilate, losartan potassium and hydrochlorothiazide in tablet dosage form. The first UV spectrophotometric method was a determination using the simultaneous equation method at 236.5, 254 and 271 nm over the concentration range 5-25, 10-50 and 5-25 μg/ml for amlodipine besilate, losartan potassium and hydrochlorothiazide, respectively. The second UV method was a determination using the area under curve method at 231.5-241.5, 249-259 and 266-276 nm over the concentration range of 5-25, 5-25 and 10-50 μg/ml for amlodipine besilate, hydrochlorothiazide and losartan potassium, respectively. In reverse phase high performance liquid chromatography analysis is carried out using 0.025 M phosphate buffer (pH 3.7):acetonitrile (57:43 v/v) as the mobile phase and Kromasil C18 (4.6 mm i.d×250 mm) column as stationery phase with detection wavelength of 232 nm linearity was obtained in the concentration range of 2-14, 20-140 and 5-40 μg/ml for amlodipine besilate, losartan potassium and hydrochlorothiazide, respectively. Both UV-spectrophotometric and reverse phase high performance liquid chromatography methods were statistically validated and can be used for analysis of combined dose tablet formulation containing amlodipine besilate, losartan potassium and hydrochlorothiazide. PMID:20582208
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Image registration for a UV-Visible dual-band imaging system
NASA Astrophysics Data System (ADS)
Chen, Tao; Yuan, Shuang; Li, Jianping; Xing, Sheng; Zhang, Honglong; Dong, Yuming; Chen, Liangpei; Liu, Peng; Jiao, Guohua
2018-06-01
The detection of corona discharge is an effective way for early fault diagnosis of power equipment. UV-Visible dual-band imaging can detect and locate corona discharge spot at all-weather condition. In this study, we introduce an image registration protocol for this dual-band imaging system. The protocol consists of UV image denoising and affine transformation model establishment. We report the algorithm details of UV image preprocessing, affine transformation model establishment and relevant experiments for verification of their feasibility. The denoising algorithm was based on a correlation operation between raw UV images, a continuous mask and the transformation model was established by using corner feature and a statistical method. Finally, an image fusion test was carried out to verify the accuracy of affine transformation model. It has proved the average position displacement error between corona discharge and equipment fault at different distances in a 2.5m-20 m range are 1.34 mm and 1.92 mm in the horizontal and vertical directions, respectively, which are precise enough for most industrial applications. The resultant protocol is not only expected to improve the efficiency and accuracy of such imaging system for locating corona discharge spot, but also supposed to provide a more generalized reference for the calibration of various dual-band imaging systems in practice.
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Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.
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Zhang, Chunhui; Ning, Ke; Zhang, Wenwen; Guo, Yuanjie; Chen, Jun; Liang, Chen
2013-04-01
Increased attention is currently being directed towards the potential negative effects of antibiotics and other PPCPs discharged into the aquatic environment via municipal WWTP secondary effluents. A number of analytical methods, such as high performance liquid chromatography technologies, including a high performance liquid chromatography-fluorescence method (HPLC-FLD), high performance liquid chromatography-UV detection method (HPLC-UV) and high performance liquid chromatography-mass spectrometry method (HPLC-MS), have been suggested as determination technologies for antibiotic residues in water. In this study, we implement a HPLC-MS/MS combined method to detect and analyze antibiotics in WWTP secondary effluent and apply a horizontal subsurface flow constructed wetland (CW) as an advanced wastewater treatment for removing antibiotics in the WWTP secondary effluent. The results show that there were 2 macrolides, 2 quinolones and 5 sulfas in WWTP secondary effluent among all the 22 antibiotics considered. After the CW advanced treatment, the concentration removal efficiencies and removal loads of 9 antibiotics were 53-100% and 0.004-0.7307 μg m(-2) per day, respectively.
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Capability of detecting ultraviolet counterparts of gravitational waves with GLUV
NASA Astrophysics Data System (ADS)
Ridden-Harper, Ryan; Tucker, B. E.; Sharp, R.; Gilbert, J.; Petkovic, M.
2017-12-01
With the discovery of gravitational waves (GWs), attention has turned towards detecting counterparts to these sources. In discussions on counterpart signatures and multimessenger follow-up strategies to the GW detections, ultraviolet (UV) signatures have largely been neglected, due to UV facilities being limited to SWIFT, which lacks high-cadence UV survey capabilities. In this paper, we examine the UV signatures from merger models for the major GW sources, highlighting the need for further modelling, while presenting requirements and a design for an effective UV survey telescope. Using the u΄-band models as an analogue, we find that a UV survey telescope requires a limiting magnitude of m_{u^' }}(AB)≈ 24 to fully complement the aLIGO range and sky localization. We show that a network of small, balloon-based UV telescopes with a primary mirror diameter of 30 cm could be capable of covering the aLIGO detection distance from ∼60 to 100 per cent for BNS events and ∼40 per cent for the black hole and a neutron star events. The sensitivity of UV emission to initial conditions suggests that a UV survey telescope would provide a unique data set, which can act as an effective diagnostic to discriminate between models.
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Escrig-Doménech, Aarón; Simó-Alfonso, Ernesto F; Ramis-Ramos, Guillermo
2016-08-17
A method for the simultaneous determination of the most frequently used surfactant families -linear alkyl benzenesulphonates (LAS), alkyl ether sulphates (AES), fatty alcohol ethoxylates (FAE) and oleins (soaps, fatty acid salts) - in cleaning products, has been developed. The common reversed phase octyl (C8), pentafluorophenyl and biphenyl columns were not capable of separating the anionic LAS and AES classes; however, since only LAS absorbs in the UV, these two classes were independently quantified using a C8 column and serially connected UV and ELSD detection. The best compromise to resolve the four surfactant classes and the oligomers within the classes was achieved with a C8 column and an ACN/water gradient. To enhance retention of the anionic surfactants, ammonium acetate, as an ion-pairing agent compatible with ELSD detection, was used. Also, to shift the olein peaks with respect to that of the FAE oligomers, acetic acid was used. In the optimized method, modulation of the mobile phase, using ammonium acetate during elution of LAS and AES, and acetic acid after elution of LAS and AES, was provided. Quantitation of the overlapped LAS and AES classes was achieved by using the UV detector to quantitate LAS and the ELSD to determine AES by difference. Accuracy in the determination of AES was achieved by using a quadratic model, and by correcting the predicted AES concentration according to the LAS concentration previously established using the UV chromatogram. Another approach also leading to accurate predictions of the AES concentration was to increase the AES concentrations in the samples by adding a standard solution. In the samples reinforced with AES, correction of the predicted AES concentration was not required. FAE and olein were quantified using also quadratic calibration. Copyright © 2016 Elsevier B.V. All rights reserved.
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Wang, Huiju; Song, Wenlan; Zhang, Min; Zhen, Qi; Guo, Mei; Zhang, Yida; Du, Xinzhen
2016-10-14
A novel titanium and nickel oxide composite nanosheets (TiO 2 /NiOCNSs) coating was in situ grown on a Nitinol (NiTi) wire by direct hydrothermal treatment and modified by self-assembly of trichlorophenylsilane for solid phase microextraction (SPME). TiO 2 /NiOCNSs were radially oriented and chemically bonded to the NiTi substrate with double-faced open access sites. Moreover the phenyl modified TiO 2 /NiOCNSs (TiO 2 /NiOCNSs-Ph) coating exhibited original surface supporting framework favorable for effective SPME. The extraction performance of TiO 2 /NiOCNSs-Ph coated NiTi (NiTi-TiO 2 /NiOCNSs-Ph) fiber was investigated for the concentration and detection of ultraviolet (UV) filters, polycyclic aromatic hydrocarbons (PAHs), phthalate acid esters and polychlorinated biphenyls coupled to HPLC with UV detection. The novel fiber exhibited better selectivity for UV filters and PAHs and presented greater extraction capability compared to commercial polydimethylsiloxane and polyacrylate fibers. Under the optimized conditions for SPME of UV filters, the proposed method presented linear ranges from 0.1 to 300μg/L with correlation coefficients of higher than 0.999 and limits of detection from 0.030μg/L to 0.064μg/L. Relative standard deviations (RSDs) were below 7.16% and 8.42% for intra-day and inter-day measurements with the single fiber, respectively. Furthermore RSDs for fiber-to-fiber reproducibility from 6.57% to 8.93% were achieved. The NiTi-TiO 2 /NiOCNSs-Ph fiber can be used up to 200 times. The proposed method was successfully applied to the preconcentration and determination of trace target UV filters in different environmental water samples. The relative recoveries from 87.3% to 104% were obtained with RSDs less than 8.7%. Copyright © 2016 Elsevier B.V. All rights reserved.
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Colorimetric detection of UV light-induced single-strand DNA breaks using gold nanoparticles.
Kim, Joong Hyun; Chung, Chan Ho; Chung, Bong Hyun
2013-02-21
We developed a colorimetric method to specifically detect single-strand DNA breaks using gold nanoparticles. In our assay, broken DNA cannot stabilize gold nanoparticles to prevent salt-induced aggregation as good as intact DNA can, and this effect can be easily observed with the naked eye as a red-to-purple color change.
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Oshima, Ryusei; Kotani, Akira; Kuroda, Minpei; Yamamoto, Kazuhiro; Mimaki, Yoshihiro; Hakamata, Hideki
2018-03-01
High-performance liquid chromatography with ultraviolet detection (HPLC-UV) using 20 mM phosphate mobile phase and an octadecylsilyl column (Triart C18, 150 × 3.0 mm i.d., 3 μm) has been developed for the analysis of hydrophilic compounds in the water extract of Schisandrae Fructus samples. The present HPLC-UV method permits the accurate and precise determination of malic, citric, and protocatechuic acids in the Japanese Pharmacopoeia (JP) Schisandrae Fructus, Schisandrae Chinensis Fructus and Schisandrae Sphenantherae Fructus. The JP Schisandrae Fructus studied contains 27.98 mg/g malic, 107.08 mg/g citric, and 0.42 mg/g protocatechuic acids, with a relative standard deviation (RSD) of repeatability of <0.9% (n = 6). The content of malic acids in Schisandrae Chinensis Fructus is approximately ten times that in Schisandrae Sphenantherae Fructus. To examine whether the HPLC-UV method is applicable to the fingerprint-based discrimination of Schisandrae Fructus samples obtained from Chinese markets, principal component analysis (PCA) was performed using the determined contents of organic acids and the ratio of six characteristic unknown peaks derived from hydrophilic components to internal standard peak areas. On the score plots, Schisandrae Chinensis Fructus and Schisandrae Sphenantherae Fructus samples are clearly discriminated. Therefore, the HPLC-UV method for the analysis of hydrophilic components coupled with PCA has been shown to be practical and useful in the quality control of Schisandrae Fructus.
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Wang, Huazi; Hu, Lu; Liu, Xinya; Yin, Shujun; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang
2017-09-22
In the present study, a simple and rapid sample preparation method designated ultrasound-assisted dispersive liquid-liquid microextraction based on a deep eutectic solvent (DES) followed by high-performance liquid chromatography with ultraviolet (UV) detection (HPLC-UVD) was developed for the extraction and determination of UV filters from water samples. The model analytes were 2,4-dihydroxybenzophenone (BP-1), benzophenone (BP) and 2-hydroxy-4-methoxybenzophenone (BP-3). The hydrophobic DES was prepared by mixing trioctylmethylammonium chloride (TAC) and decanoic acid (DecA). Various influencing factors (selection of the extractant, amount of DES, ultrasound duration, salt addition, sample volume, sample pH, centrifuge rate and duration) on UV filter recovery were systematically investigated. Under optimal conditions, the proposed method provided good recoveries in the range of 90.2-103.5% and relative standard deviations (inter-day and intra-day precision, n=5) below 5.9%. The enrichment factors for the analytes ranged from 67 to 76. The limits of detection varied from 0.15 to 0.30ngmL -1 , depending on the analytes. The linearities were between 0.5 and 500ngmL -1 for BP-1 and BP and between 1 and 500ngmL -1 for BP-3, with coefficients of determination greater than 0.99. Finally, the proposed method was applied to the determination of UV filters in swimming pool and river water samples, and acceptable relative recoveries ranging from 82.1 to 106.5% were obtained. Copyright © 2017. Published by Elsevier B.V.
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Cetin, Sevil Müge; Atmaca, Sedef
2004-03-26
A simple and reliable high-performance liquid chromatographic (HPLC) method with UV-Vis detection has been developed and validated for the determination of vigabatrin (VG) in human plasma and urine. The samples were pre-column derivatizated with 1,2-naphthoquinone-4-sulphonic acid sodium salt (NQS). A good chromatographic separation was achieved on a C18 column with a mobile phase consisting of acetonitrile and 10 mM orthophosphoric acid (pH 2.5) gradient elution. Tranexamic acid was used as an internal standard (I.S.). The method was linear over the concentration range of 0.8-30.0 microg/ml for both samples. The method is precise (relative standard deviation (R.S.D.) <9.13%) and accurate (relative mean error (RME) <-8.75%); analytical recoveries were 81.07% for plasma and 83.05% for urine. The assay was applied to pharmacokinetic study in a healthy volunteer after a single oral administration of 1 g of vigabatrin.
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Huang, Zhuo; Ito, Kazuaki; Hirokawa, Takeshi
2004-11-05
A novel, simple and highly sensitive CE method was developed to determine total iodine (TI) in seawater. The method is based on the on-capillary reduction of iodine species to iodide by a reductant, introduced into the capillary before sample injection, the preconcentration of iodide using isotachophoresis, followed by its UV detection. Under optimized conditions for reduction and CE separation, the limit of detection for TI (S/N = 3) reached 0.4 microg L(-1) (226 nm). The repeatability of migration time and peak area, expressed by relative standard deviation, was 0.46 and 1.45%, respectively (n = 19). The correlation factor was 0.9991 (n = 10) for the concentration range of 12-115 microg I L(-1). The CE results obtained for the real seawater analysis agreed with the data of ion chromatography. To determine the genuine TI by the proposed method, organic iodinated compounds in the sample were treated with H202 and irradiation with UV light before analysis.
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Zhou, M; Miles, C J
1991-01-01
Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.
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De Paoli, Giorgia; Brandt, Simon D; Wallach, Jason; Archer, Roland P; Pounder, Derrick J
2013-06-01
Three psychoactive arylcyclohexylamines, advertised as "research chemicals," were obtained from an online retailer and characterized by gas chromatography ion trap electron and chemical ionization mass spectrometry, nuclear magnetic resonance spectroscopy and diode array detection. The three phencyclidines were identified as 2-(ethylamino)-2-(3-methoxyphenyl)cyclohexanone (methoxetamine), N-ethyl-1-(3-methoxyphenyl)cyclohexanamine and 1-[1-(3-methoxyphenyl)cyclohexyl]piperidine. A qualitative/quantitative method of analysis was developed and validated using liquid chromatography (HPLC) electrospray tandem mass spectrometry and ultraviolet (UV) detection for the determination of these compounds in blood, urine and vitreous humor. HPLC-UV proved to be a robust, accurate and precise method for the qualitative and quantitative analysis of these substances in biological fluids (0.16-5.0 mg/L), whereas the mass spectrometer was useful as a confirmatory tool.
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Online in-tube microextractor coupled with UV-Vis spectrophotometer for bisphenol A detection.
Poorahong, Sujittra; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya
2013-01-01
A simple and high extraction efficiency online in-tube microextractor (ITME) was developed for bisphenol A (BPA) detection in water samples. The ITME was fabricated by a stepwise electrodeposition of polyaniline, polyethylene glycol and polydimethylsiloxane composite (CPANI) inside a silico-steel tube. The obtained ITME coupled with UV-Vis detection at 278 nm was investigated. By this method, the extraction and pre-concentration of BPA in water were carried out in a single step. Under optimum conditions, the system provided a linear dynamic range of 0.1 to 100 μM with a limit of detection of 20 nM (S/N ≥3). A single in-tube microextractor had a good stability of more than 60 consecutive injections for 10.0 μM BPA with a relative standard deviation of less than 4%. Moreover, a good tube-to-tube reproducibility and precision were obtained. The system was applied to detect BPA in water samples from six brands of baby bottles and the results showed good agreement with those obtained from the conventional GC-MS method. Acceptable percentage recoveries from the spiked water samples were obtained, ranging from 83-102% for this new method compared with 73-107% for the GC-MS standard method. This new in-tube CPANI microextractor provided an excellent extraction efficiency and a good reproducibility. In addition, it can also be easily applied for the analysis of other polar organic compounds contaminated in water sample.
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UV plasmonic device for sensing ethanol and acetone
NASA Astrophysics Data System (ADS)
Honda, Mitsuhiro; Ichikawa, Yo; Rozhin, Alex G.; Kulinich, Sergei A.
2018-01-01
In the present study, we demonstrate efficient detection of volatile organic vapors with improved sensitivity, exploiting the localized surface plasmon resonance of indium nanograins in the UV range (UV-LSPR). The sensitivity of deep-UV-LSPR measurements toward ethanol was observed to be 0.004 nm/ppm, which is 10 times higher than that of a previously reported visible-LSPR device based on Ag nanoprisms [Sensors 11, 8643 (2011)]. Although practical issues such as improving detection limits are still remaining, the results of the present study suggest that the new approach based on UV-LSPR may open new avenues to the detection of organic molecules in solid, liquid, and gas phases using plasmonic sensors.
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UV-sensitive scientific CCD image sensors
NASA Astrophysics Data System (ADS)
Vishnevsky, Grigory I.; Kossov, Vladimir G.; Iblyaminova, A. F.; Lazovsky, Leonid Y.; Vydrevitch, Michail G.
1997-06-01
An investigation of probe laser irradiation interaction with substances containing in an environment has long since become a recognized technique for contamination detection and identification. For this purpose, a near and midrange-IR laser irradiation is traditionally used. However, as many works presented on last ecology monitoring conferences show, in addition to traditional systems, rapidly growing are systems with laser irradiation from near-UV range (250 - 500 nm). Use of CCD imagers is one of the prerequisites for this allowing the development of a multi-channel computer-based spectral research system. To identify and analyze contaminating impurities on an environment, such methods as laser fluorescence analysis, UV absorption and differential spectroscopy, Raman scattering are commonly used. These methods are used to identify a large number of impurities (petrol, toluene, Xylene isomers, SO2, acetone, methanol), to detect and identify food pathogens in real time, to measure a concentration of NH3, SO2 and NO in combustion outbursts, to detect oil products in a water, to analyze contaminations in ground waters, to define ozone distribution in the atmosphere profile, to monitor various chemical processes including radioactive materials manufacturing, heterogeneous catalytic reactions, polymers production etc. Multi-element image sensor with enhanced UV sensitivity, low optical non-uniformity, low intrinsic noise and high dynamic range is a key element of all above systems. Thus, so called Virtual Phase (VP) CCDs possessing all these features, seems promising for ecology monitoring spectral measuring systems. Presently, a family of VP CCDs with different architecture and number of pixels is developed and being manufactured. All CCDs from this family are supported with a precise slow-scan digital image acquisition system that can be used in various image processing systems in astronomy, biology, medicine, ecology etc. An image is displayed directly on a PC monitor through a software support.
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Tavallali, Hossein; Deilamy-Rad, Gohar; Parhami, Abolfath; Kiyani, Sajede
2014-01-01
A new selective chemodosimeter probe was developed by the introduction of dithizone (DTZ) as a simple and available dye for detection of cyanide in aqueous media which enables recognition of cyanide over other competing anions such as acetate, dihydrogen phosphate, fluoride and benzoate through covalent bonding. The sensing properties of DTZ were investigated in DMSO/H2O (1:9) and have demonstrated a very high selectivity toward the cyanide anions. A reasonable recognition mechanism was suggested using UV-Vis, (1)H NMR and FTIR spectroscopy techniques. Time dependent density function theory (TDDFT) computations of UV-Vis excitation for DTZ2-CN adduct agreed well with our experimental findings. The detection limit of the new chromogenic probe was measured to be 0.48 μmol L(-1) which is much lower than most recently reported chromogenic probes for cyanide determination. The analytical utility of the method for the analysis of cyanide ions in electroplating wastewater (EPWW), human serum, tap and mineral water samples was demonstrated and the results were compared successfully with the conventional reference method. The short time response and the detection by the naked eye make the method available for the detection and quantitative determination of cyanide in a variety of real samples. Copyright © 2013 Elsevier B.V. All rights reserved.
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Wojtecki, Rudy J; Yuen, Alexander Y; Zimmerman, Thomas G; Jones, Gavin O; Horn, Hans W; Boday, Dylan J; Hedrick, James L; García, Jeannette M
2015-08-07
The detection of trace amounts (<10 ppb) of heavy metals in aqueous solutions is described using 1,3,5-hexahydro-1,3,5-triazines (HTs) as chemical indicators and a low cost fluorimeter-based detection system. This method takes advantage of the inherent properties of HTs to coordinate strongly with metal ions in solution, a fundamental property that was studied using a combination of analytical tools (UV-Vis titrations, (1)H-NMR titrations and computational modeling). Based on these fundamental studies that show significant changes in the HT UV signature when a metal ion is present, HT compounds were used to prepare indicator strips that resulted in significant fluorescence changes when a metal was present. A portable and economical approach was adopted to test the concept of utilizing HTs to detect heavy metals using a fluorimeter system that consisted of a low-pressure mercury lamp, a photo-detector, a monolithic photodiode and an amplifier, which produces a voltage proportional to the magnitude of the visible fluorescence emission. Readings of the prepared HT test strips were evaluated by exposure to two different heavy metals at the safe threshold concentration described by the U.S. Environmental Protection Agency (EPA) for Cr(3+) and Ag(2+) (100 μg L(-1) and 6.25, respectively). This method of detection could be used to the presence of either metal at these threshold concentrations.
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On-site comprehensive analysis of explosives using HPLC-UV-PAED
NASA Astrophysics Data System (ADS)
Marple, Ronita L.; LaCourse, William R.
2004-03-01
High-performance liquid chromatography with ultra violet and photo-assisted electrochemical detection (HPLC-UV-PAED) has been developed for the sensitive and selective detection of explosives in ground water and soil extracts. Fractionation and preconcentration of explosives is accomplished with on-line solid phase extraction (SPE), which minimizes sample pretreatment and enables faster and more accurate on-site assessment of a contaminated site. Detection limits are equivalent or superior (i.e., <1 part-per-trillion for HMX) to those achieved using the Environmental Protection Agency (EPA) Method 8330. This approach is more broadly applicable, as it is capable of determining a wider range of organic nitro compounds. Soil samples are extracted using pressurized fluid extraction (PFE), and this technique is automatable, field-compatible, and environmentally friendly, adding to the overall efficiency of the methodology.
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Ramkumar, Abilasha; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon
2012-08-15
The present study demonstrates a simple, rapid and efficient method for the determination of chlorinated anilines (CAs) in environmental water samples using ultrasonication assisted emulsification microextraction technique based on solidification of floating organic droplet (USAEME-SFO) coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection. In this extraction method, 1-dodecanol was used as extraction solvent which is of lower density than water, low toxicity, low volatility, and low melting point (24 °C). After the USAEME, extraction solvent could be collected easily by keeping the extraction tube in ice bath for 2 min and the solidified organic droplet was scooped out using a spatula and transferred to another glass vial and allowed to thaw. Then, 10 μL of extraction solvent was diluted with mobile phase (1:1) and taken for HPLC-UV analysis. Parameters influencing the extraction efficiency, such as the kind and volume of extraction solvent, volume of sample, ultrasonication time, pH and salt concentration were thoroughly examined and optimized. Under the optimal conditions, the method showed good linearity in the concentration range of 0.05-500 ng mL(-1) with correlation coefficients ranging from 0.9948 to 0.9957 for the three target CAs. The limit of detection based on signal to noise ratio of 3 ranged from 0.01 to 0.1 ng mL(-1). The relative standard deviations (RSDs) varied from 2.1 to 6.1% (n=3) and the enrichment factors ranged from 44 to 124. The proposed method has also been successfully applied to analyze real water samples and the relative recoveries of environmental water samples ranged from 81.1 to 116.9%. Copyright © 2012 Elsevier B.V. All rights reserved.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Rastogi, Rajesh P.; Laboratory of Photobiology and Molecular Microbiology, Centre of Advanced Study in Botany, Banaras Hindu University, Varanasi 221005; Singh, Shailendra P.
2010-07-02
The generation of reactive oxygen species (ROS) under simulated solar radiation (UV-B: 0.30 Wm{sup -2}, UV-A: 25.70 Wm{sup -2} and PAR: 118.06 Wm{sup -2}) was studied in the cyanobacterium Anabaena variabilis PCC 7937 using the oxidant-sensing fluorescent probe 2',7'-dichlorodihydrofluorescein diacetate (DCFH-DA). DCFH-DA is a nonpolar dye, converted into the polar derivative DCFH by cellular esterases that are nonfluorescent but switched to highly fluorescent DCF when oxidized by intracellular ROS and other peroxides. The images obtained from the fluorescence microscope after 12 h of irradiation showed green fluorescence from cells covered with 295, 320 or 395 nm cut-off filters, indicating themore » generation of ROS in all treatments. However, the green/red fluorescence ratio obtained from fluorescence microscopic analysis showed the highest generation of ROS after UV-B radiation in comparison to PAR or UV-A radiation. Production of ROS was also measured by a spectrofluorophotometer and results obtained supported the results of fluorescence microscopy. Low levels of ROS were detected at the start (0 h) of the experiment showing that they are generated even during normal metabolism. This study also showed that UV-B radiation causes the fragmentation of the cyanobacterial filaments which could be due to the observed oxidative stress. This is the first report for the detection of intracellular ROS in a cyanobacterium by fluorescence microscopy using DCFH-DA and thereby suggesting the applicability of this method in the study of in vivo generation of ROS.« less
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Zhen, Qi; Zhang, Min; Song, Wenlan; Wang, Huiju; Wang, Xuemei; Du, Xinzhen
2016-10-01
An oriented titanium-nickel oxide composite nanotubes coating was in situ grown on a nitinol wire by direct electrochemical anodization in ethylene glycol with ammonium fluoride and water for the first time. The morphology and composition of the resulting coating showed that the anodized nitinol wire provided a titania-rich coating. The titanium-nickel oxide composite nanotubes coated fiber was used for solid-phase microextraction of different aromatic compounds coupled to high-performance liquid chromatography with UV detection. The titanium-nickel oxide composite nanotubes coating exhibited high extraction capability, good selectivity, and rapid mass transfer for weakly polar UV filters. Thereafter the important parameters affecting extraction efficiency were investigated for solid-phase microextraction of UV filters. Under the optimized conditions, the calibration curves were linear in the range of 0.1-300 μg/L for target UV filters with limits of detection of 0.019-0.082 μg/L. The intraday and interday precision of the proposed method with the single fiber were 5.3-7.2 and 5.9-7.9%, respectively, and the fiber-to-fiber reproducibility ranged from 6.3 to 8.9% for four fibers fabricated in different batches. Finally, its applicability was evaluated by the extraction and determination of target UV filters in environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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UV-Visible Spectroscopic Method and Models for Assessment and Monitoring of Harmful Algal Blooms
NASA Technical Reports Server (NTRS)
Mitchell, B. Greg
2000-01-01
The development of an enhanced predictive and early warning capability for the occurrence and impact of harmful algal blooms (HABs) would be of great benefit to coastal communities. A critical issue for early detection and monitoring of HABs is the need to detect harmful algal species within a mixed-species phytoplankton assemblage. Possession of UV-absorbing compounds called mycosporine-like amino acids (MAAs) may be one factor that allows HAB species to out-compete their phytoplankton neighbors. Possession of MAAs, which we believe can be inferred from strong UV-absorption signals in phytoplankton absorption coefficients, can be used as a flag for potential HAB outbreak. The goal of this project was to develop a solar simulating UV-visible incubator to grow HAB dinoflagellates, to begin MAA analysis of samples collected on global cruises, and to carry out initial experiments on HAB dinoflagellate species in pure culture. Our scientific objectives are to quantify MAA production and spectral induction mechanisms in HAB species, to characterize spectral absorption of MAAs, and to define the ecological benefit of MAAs (i.e. photoprotection). Data collected on cruises to the global oceans will be used to parameterize phytoplankton absorption in the UV region, and this parameterization could be incorporated into existing models of seawater optical properties in the UV spectral region. Data collected in this project were used for graduate fellowship applications by Elizabeth Frame. She has been awarded an EPA STAR fellowship to continue the work initiated by this project.
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Soares, M E; Carvalho, M; Carmo, H; Remião, F; Carvalho, F; Bastos, M L
2004-03-01
Amphetamine derivatives are a class of compounds increasingly abused as recreational drugs in various regions of the world. Although d-amphetamine (AMPH) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) are among the most commonly used, the abuse of other designer drugs such as 4-bromo-2,5-dimethoxyphenethylamine (2C-B) and 4-methylthioamphetamine (4-MTA) and their involvement in acute intoxications has been increasingly reported. There is evidence that abusers ingest these compounds either alone or in combination and the respective monitoring is important for both legal and health care purposes in hospital emergency. In the present study a simple and clean solid-phase extraction procedure from urine of AMPH and MDMA, and their major metabolites p-hydroxyamphetamine (OH-AMPH) and methylenedioxyamphetamine (MDA) and 2C-B and 4-MTA was developed. Analysis was performed by HPLC-UV and the precision of the technique was between 2.9 and 5.3% for all compounds. For the overall procedure, the precision values were between 3.3 and 5.9%. Recoveries obtained from spiked urines at three concentration levels were better than 84 +/- 4% for the six compounds. The limit of detection of the method for the compounds (between 5.3 and 84.0 ng) enables their identification in urine after ingestion of fatal and non-fatal doses. The main advantages of the present method lie in its simple, clean and reliable SPE extraction method of the six amphetamine derivatives from urine followed by their simultaneous detection and quantification by liquid chromatography with UV detection. Copyright 2004 John Wiley & Sons, Ltd.
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Bias Selectable Dual Band AlGaN Ultra-violet Detectors
NASA Technical Reports Server (NTRS)
Yan, Feng; Miko, Laddawan; Franz, David; Guan, Bing; Stahle, Carl M.
2007-01-01
Bias selectable dual band AlGaN ultra-violet (UV) detectors, which can separate UV-A and UV-B using one detector in the same pixel by bias switching, have been designed, fabricated and characterized. A two-terminal n-p-n photo-transistor-like structure was used. When a forward bias is applied between the top electrode and the bottom electrode, the detectors can successfully detect W-A and reject UV-B. Under reverse bias, they can detect UV-B and reject UV-A. The proof of concept design shows that it is feasible to fabricate high performance dual-band UV detectors based on the current AlGaN material growth and fabrication technologies.
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Chen, Xingxing; Wu, Xiaoli; Gan, Min; Xu, Feng; He, Lihua; Yang, Dong; Xu, Hengyi; Shah, Nagendra P; Wei, Hua
2015-03-01
Staphylococcus aureus is one of the main pathogens in dairy and meat products; therefore, developing a highly sensitive and rapid method for its detection is necessary. In this study, a quantitative detection method for Staph. aureus was developed using silica-coated magnetic nanoparticles and thermophilic helicase-dependent isothermal amplification. First, genomic DNA was extracted from lysed bacteria using silica-coated magnetic nanoparticles and amplified using thermophilic helicase-dependent isothermal amplification. After adding the nucleic-acid dye SYBR Green I to the amplicons, the fluorescence intensity was observed using a UV lamp or recorded using a fluorescence spectrophotometer. This detection system had a detection limit of 5×10(0) cfu/mL in pure culture and milk-powder samples and 5×10(1) cfu/mL in pork samples using a UV light in less than 2h. In addition, a good linear relationship was obtained between fluorescence intensity and bacterial concentrations ranging from 10(2) to 10(4) cfu/mL under optimal conditions. Furthermore, the results from contaminated milk powder and pork samples suggested that the detection system could be used for the quantitative analysis of Staph. aureus and applied potentially to the food industry for the detection of this pathogen. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.
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Invisible ink mark detection in the visible spectrum using absorption difference.
Lee, Joong; Kong, Seong G; Kang, Tae-Yi; Kim, Byounghyun; Jeon, Oc-Yeub
2014-03-01
One of popular techniques in gambling fraud involves the use of invisible ink marks printed on the back surface of playing cards. Such covert patterns are transparent in the visible spectrum and therefore invisible to unaided human eyes. Invisible patterns can be made visible with ultraviolet (UV) illumination or a CCD camera installed with an infrared (IR) filter depending on the type of ink materials used. Cheating gamers often wear contact lenses or eyeglasses made of IR or UV filters to recognize the secret marks on the playing cards. This paper presents an image processing technique to reveal invisible ink patterns in the visible spectrum without the aid of special equipment such as UV lighting or IR filters. A printed invisible ink pattern leaves a thin coating on the surface with different refractive index for different wavelengths of light, which results in color dispersion or absorption difference. The proposed method finds the differences of color components caused by absorption difference to detect invisible ink patterns on the surface. Experiment results show that the proposed scheme is effective for both UV-active and IR-active invisible ink materials. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.
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Barta, András; Horváth, Gábor
2004-02-21
The perception of skylight polarization in the ultraviolet (UV) by many insect species for orientation purposes is rather surprising, because both the degree of linear polarization and the radiance of light from the clear sky are considerably lower in the UV than in the blue or green. In this work we call this the "UV-sky-pol paradox". Although in the past, several attempts have been made to resolve this paradox, none of them was convincing. We present here a possible quantitative resolution to the paradox. We show by a model calculation that if the air layer between a cloud and a ground-based observer is partly sunlit, the degree of linear polarization p of skylight originating from the cloudy region is highest in the UV, because in this spectral range the unpolarized UV-deficient cloudlight dilutes least the polarized light scattered in the air beneath the cloud. Similarly, if the air under foliage is partly sunlit, p of downwelling light from the canopied region is maximal in the UV, because in this part of spectrum the unpolarized UV-deficient green canopylight dilutes least the polarized light scattered in the air beneath the canopy. Therefore, the detection of polarization of downwelling light under clouds or canopies is most advantageous in the UV, in which spectral range the risk is the smallest that the degree of polarization p is lower than the threshold p(tr) of polarization sensitivity in animals. On the other hand, under clear skies there is no favoured wavelength for perception of celestial polarization, because p of skylight is high enough (p > p(tr)) at all wavelengths. We show that there is an analogy between the detection of UV skylight polarization and the polarotactic water detection in the UV. However, insects perceive skylight polarization by UV or blue or green receptors. The question, why they differ in the spectral channel used for the detection of celestial polarization cannot be answered at the present time, because data are insufficient. Nevertheless, we present here one possible atmospheric optical reason why certain visual systems involved in detecting celestial polarization, are specifically tuned to the UV part of the spectrum.
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Application of ZnO Nanoparticle as Sulphide Gas Sensor Using UV/VIS/NIR-Spectrophotometer
NASA Astrophysics Data System (ADS)
Juliasih, N.; Buchari; Noviandri, I.
2017-04-01
The nanoparticle of metal oxides has great unique characteristics that applicable to the wide industrial as sensors and catalysts for reducing environmental pollution. Sulphide gas monitors and detectors are required for assessing safety aspects, due to its toxicity level. A thin film of ZnO as the sulphide gas sensor was synthesised by the simple method of chemical liquid deposition with variation of annealing temperature from 200 ºC to 500 ºC, and characterised by Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), and UV/VIS/NIR-Spectrophotometer. Characterization studies showed nanoparticle size from the range 62 - 92 nm of diameters. The application this ZnO thin film to sulfide gas, detected by UV/VIS/NIR Spectrophotometer with diffuse reflectance, showed specific chemical reaction by the shifting of maximum % Reflectance peak. The gas sensing using this method is applicable at room.
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Valente, T A M; Silva, D M; Gomes, P S; Fernandes, M H; Santos, J D; Sencadas, V
2016-02-10
Medically approved sterility methods should be a major concern when developing a polymeric scaffold, mainly when commercialization is envisaged. In the present work, poly(lactic acid) (PLA) fiber membranes were processed by electrospinning with random and aligned fiber alignment and sterilized under UV, ethylene oxide (EO), and γ-radiation, the most common ones for clinical applications. It was observed that UV light and γ-radiation do not influence fiber morphology or alignment, while electrospun samples treated with EO lead to fiber orientation loss and morphology changing from cylindrical fibers to ribbon-like structures, accompanied to an increase of polymer crystallinity up to 28%. UV light and γ-radiation sterilization methods showed to be less harmful to polymer morphology, without significant changes in polymer thermal and mechanical properties, but a slight increase of polymer wettability was detected, especially for the samples treated with UV radiation. In vitro results indicate that both UV and γ-radiation treatments of PLA membranes allow the adhesion and proliferation of MG 63 osteoblastic cells in a close interaction with the fiber meshes and with a growth pattern highly sensitive to the underlying random or aligned fiber orientation. These results are suggestive of the potential of both γ-radiation sterilized PLA membranes for clinical applications in regenerative medicine, especially those where customized membrane morphology and fiber alignment is an important issue.
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NASA Astrophysics Data System (ADS)
El-Nour, K. M. A.; Salam, E. T. A.; Soliman, H. M.; Orabi, A. S.
2017-03-01
A new optical sensor was developed for rapid screening with high sensitivity for the existence of biogenic amines (BAs) in poultry meat samples. Gold nanoparticles (GNPs) with particle size 11-19 nm function as a fast and sensitive biosensor for detection of histamine resulting from bacterial decarboxylation of histidine as a spoilage marker for stored poultry meat. Upon reaction with histamine, the red color of the GNPs converted into deep blue. The appearance of blue color favorably coincides with the concentration of BAs that can induce symptoms of poisoning. This biosensor enables a semi-quantitative detection of analyte in real samples by eye-vision. Quality evaluation is carried out by measuring histamine and histidine using different analytical techniques such as UV-vis, FTIR, and fluorescence spectroscopy as well as TEM. A rapid quantitative readout of samples by UV-vis and fluorescence methods with standard instrumentation were proposed in a short time unlike chromatographic and electrophoretic methods. Sensitivity and limit of detection (LOD) of 6.59 × 10-4 and 0.6 μM, respectively, are determined for histamine as a spoilage marker with a correlation coefficient ( R 2) of 0.993.
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Douki, T; Voituriez, L; Cadet, J
1995-03-01
Pyrimidine (6-4) pyrimidone photoproducts constitute one of the major classes of DNA lesions induced by far-UV irradiation. However, their biological role remains difficult to assess partly because of the lack of a specific and sensitive assay for monitoring their formation in DNA. Here is presented a measurement method based on the release of the (6-4) base adducts from DNA followed by an HPLC separation associated with a sensitive and specific fluorescence detection. The quantitative and mechanistic aspects of the chemical hydrolysis, based on the use of hydrogen fluoride stabilized in pyridine, were investigated, using dinucleoside monophosphate (6-4) photoproducts as model compounds. The final hydrolysis products were isolated and characterized by UV, fluorescence, mass, and 1H NMR spectroscopies. Application of the assay to far-UV irradiated calf thymus DNA provided information on the sequence effect on the rate of formation of three of the four possible bipyrimidine (6-4) photoproducts.
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Wang, Heye; Dou, Peng; Lü, Chenchen; Liu, Zhen
2012-07-13
Erythropoietin (EPO) is an important glycoprotein hormone. Recombinant human EPO (rhEPO) is an important therapeutic drug and can be also used as doping reagent in sports. The analysis of EPO glycoforms in pharmaceutical and sports areas greatly challenges analytical scientists from several aspects, among which sensitive detection and effective and facile sample preparation are two essential issues. Herein, we investigated new possibilities for these two aspects. Deep UV laser-induced fluorescence detection (deep UV-LIF) was established to detect the intrinsic fluorescence of EPO while an immuno-magnetic beads-based extraction (IMBE) was developed to specifically extract EPO glycoforms. Combined with capillary zone electrophoresis (CZE), CZE-deep UV-LIF allows high resolution glycoform profiling with improved sensitivity. The detection sensitivity was improved by one order of magnitude as compared with UV absorbance detection. An additional advantage is that the original glycoform distribution can be completely preserved because no fluorescent labeling is needed. By combining IMBE with CZE-deep UV-LIF, the overall detection sensitivity was 1.5 × 10⁻⁸ mol/L, which was enhanced by two orders of magnitude relative to conventional CZE with UV absorbance detection. It is applicable to the analysis of pharmaceutical preparations of EPO, but the sensitivity is insufficient for the anti-doping analysis of EPO in blood and urine. IMBE can be straightforward and effective approach for sample preparation. However, antibodies with high specificity were the key for application to urine samples because some urinary proteins can severely interfere the immuno-extraction. Copyright © 2012 Elsevier B.V. All rights reserved.
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Wang, Jianling; Xiao, Xiaofeng; Chen, Tong; Liu, Tingfei; Tao, Huaming; He, Jun
2016-06-17
The glyceride in oil food simulant usually causes serious interferences to target analytes and leads to failure of the normal function of the RP-HPLC column. In this work, a convenient HPLC-UV method for the determination of the total specific migration of nine ultraviolet (UV) absorbers in food simulants was developed based on 1,1,3,3-tetramethylguanidine (TMG) and organic phase anion exchange (OPAE) SPE to efficiently remove glyceride in olive oil simulant. In contrast to the normal ion exchange carried out in an aqueous solution or aqueous phase environment, the OPAE SPE was performed in the organic phase environments, and the time-consuming and challenging extraction of the nine UV absorbers from vegetable oil with aqueous solution could be readily omitted. The method was proved to have good linearity (r≥0.99992), precision (intra-day RSD≤3.3%), and accuracy(91.0%≤recoveries≤107%); furthermore, the lower limit of quantifications (0.05-0.2mg/kg) in five types of food simulants(10% ethanol, 3% acetic acid, 20% ethanol, 50% ethanol and olive oil) was observed. The method was found to be well suited for quantitative determination of the total specific migration of the nine UV absorbers both in aqueous and vegetable oil simulant according to Commission Regulation (EU) No. 10/2011. Migration levels of the nine UV absorbers were determined in 31 plastic samples, and UV-24, UV-531, HHBP and UV-326 were frequently detected, especially in olive oil simulant for UV-326 in PE samples. In addition, the OPAE SPE procedure was also been applied to efficiently enrich or purify seven antioxidants in olive oil simulant. Results indicate that this procedure will have more extensive applications in the enriching or purification of the extremely weak acidic compounds with phenol hydroxyl group that are relatively stable in TMG n-hexane solution and that can be barely extracted from vegetable oil. Copyright © 2016 Elsevier B.V. All rights reserved.
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Hosseini, SM; Azar-Daryany, MK; Massudi, R; Elikaei, A
2011-01-01
Background The aim of this study was to investigate the effect of pulsed ultra-violet (UV) irradiation on inactivation of beer spoilage microorganisms. UV irradiation is nowadays cost effective enough to compete with traditional biological, physical, and chemical treatment technologies and has become an alternative to such methods. Material and Methods Photoinactivation effects of pulsed UV laser with the wavelengths of 355 and 266 nm, which inactivate typical prokaryotic (Escherichia coli) and eukaryotic (Saccharomyces cerevisiae) microorganisms, were examined with different doses and exposure times. Results A dose of 100 J/cm2 of the 355 nm pulsed UV laser was able to reduce about 1 to 2 log (88.75%) of E.coli with the population of 1.6×108 colony-forming units (CFU/ml), and 97% of 3.2×107, 3×106, 5.5×105, and 9×104 CFU/ml. In the case of 266 nm, more than 99% reduction in E. coli serial dilutions was inactivated, using 10 J/cm2 with exception of 7×104 CFU/ml which was not detected any bacterial growth using 5 J/cm2. In addition, 50, 40, and 20 J/cm2 energy were used successfully to inactivate S. cerevisiae at the populations of 5.4×106, 7×105, 5×104 and 4×103 CFU/ml, respectively. As a result, pulsed UV Laser with 266 nm was strong enough to inactivate a high titer of bacterial and yeast indicator standards suspended in non-alcoholic beer in comparison with 355nm doses. Conclusion Results indicate that pulsed UV technology, in principle, is an attractive alternative to conventional methods for the inactivation of indicator microorganisms and has potential in irradiation of unpasteurized beer. PMID:22347580
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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.
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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.
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Soliven, Arianne; Haidar Ahmad, Imad A; Tam, James; Kadrichu, Nani; Challoner, Pete; Markovich, Robert; Blasko, Andrei
2017-09-05
Amikacin, an aminoglycoside antibiotic lacking a UV chromophore, was developed into a drug product for delivery by inhalation. A robust method for amikacin assay analysis and aerosol particle size distribution (aPSD) determination, with comparable performance to the conventional UV detector was developed using a charged aerosol detector (CAD). The CAD approach involved more parameters for optimization than UV detection due to its sensitivity to trace impurities, non-linear response and narrow dynamic range of signal versus concentration. Through careful selection of the power transformation function value and evaporation temperature, a wider linear dynamic range, improved signal-to-noise ratio and high repeatability were obtained. The influences of mobile phase grade and glassware binding of amikacin during sample preparation were addressed. A weighed (1/X 2 ) least square regression was used for the calibration curve. The limit of quantitation (LOQ) and limit of detection (LOD) for this method were determined to be 5μg/mL and 2μg/mL, respectively. The method was validated over a concentration range of 0.05-2mg/mL. The correlation coefficient for the peak area versus concentration was 1.00 and the y-intercept was 0.2%. The recovery accuracies of triplicate preparations at 0.05, 1.0, and 2.0mg/mL were in the range of 100-101%. The relative standard deviation (S rel ) of six replicates at 1.0mg/mL was 1%, and S rel of five injections at the limit of quantitation was 4%. A robust HPLC-CAD method was developed and validated for the determination of the aPSD for amikacin. The CAD method development produced a simplified procedure with minimal variability in results during: routine operation, transfer from one instrument to another, and between different analysts. Copyright © 2017 Elsevier B.V. All rights reserved.
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Manasfi, Tarek; Coulomb, Bruno; Ravier, Sylvain; Boudenne, Jean-Luc
2017-12-05
Organic ultraviolet (UV) filters are used in sunscreens and other personal-care products to protect against harmful effects of exposure to UV solar radiation. Little is known about the fate of UV filters in seawater swimming pools disinfected with chlorine. The present study investigated the occurrence and fate of five commonly used organic UV filters, namely dioxybenzone, oxybenzone, avobenzone, 2-ethylhexyl-4-methoxycinnamate, and octocrylene, in chlorinated seawater swimming pools. Pool samples were collected to monitor the variation of UV filter concentrations during pool opening hours. Furthermore, laboratory-controlled chlorination experiments were conducted in seawater spiked with UV filters to investigate the reactivity of UV filters. Extracts of chlorination reaction samples were analyzed using high-resolution mass spectrometry and electron-capture detection to identify the potentially formed byproducts. In the collected pool samples, all the UV filters except dioxybenzone were detected. Chlorination reactions showed that only octocrylene was stable in chlorinated seawater. The four reactive UV filters generated brominated transformation products and disinfection byproducts. This formation of brominated products resulted from reactions between the reactive UV filters and bromine, which is formed rapidly when chlorine is added to seawater. Based on the identified byproducts, the transformation pathways of the reactive UV filters were proposed for the first time. Bromoform was generated by all the reactive UV filters at different yields. Bromal hydrate was also detected as one of the byproducts generated by oxybenzone and dioxybenzone.
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Lanzarotta, Adam; Lorenz, Lisa; Voelker, Sarah; Falconer, Travis M; Batson, JaCinta S
2018-05-01
This manuscript is a continuation of a recent study that described the use of fully integrated gas chromatography with direct deposition Fourier transform infrared detection and mass spectrometric detection (GC-FT-IR-MS) to identify and confirm the presence of sibutramine and AB-FUBINACA. The purpose of the current study was to employ the GC-FT-IR portion of the same instrument to quantify these compounds, thereby demonstrating the ability to identify, confirm, and quantify drug substances using a single GC-FT-IR-MS unit. The performance of the instrument was evaluated by comparing quantitative analytical figures of merit to those measured using an established, widely employed method for quantifying drug substances, high performance liquid chromatography with ultraviolet detection (HPLC-UV). The results demonstrated that GC-FT-IR was outperformed by HPLC-UV with regard to sensitivity, precision, and linear dynamic range (LDR). However, sibutramine and AB-FUBINACA concentrations measured using GC-FT-IR were not significantly different at the 95% confidence interval compared to those measured using HPLC-UV, which demonstrates promise for using GC-FT-IR as a semi-quantitative tool at the very least. The most significant advantage of GC-FT-IR compared to HPLC-UV is selectivity; a higher level of confidence regarding the identity of the analyte being quantified is achieved using GC-FT-IR. Additional advantages of using a single GC-FT-IR-MS instrument for identification, confirmation, and quantification are efficiency, increased sample throughput, decreased consumption of laboratory resources (solvents, chemicals, consumables, etc.), and thus cost.
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The research on a novel type of the solar-blind UV head-mounted displays
NASA Astrophysics Data System (ADS)
Zhao, Shun-long
2011-08-01
Ultraviolet technology of detecting is playing a more and more important role in the field of civil application, especially in the corona discharge detection, in modern society. Now the UV imaging detector is one of the most important equipments in power equipment flaws detection. And the modern head-mounted displays (HMDs) have shown the applications in the fields of military, industry production, medical treatment, entertainment, 3D visualization, education and training. We applied the system of head-mounted displays to the UV image detection, and a novel type of head-mounted displays is presented: the solar-blind UV head-mounted displays. And the structure is given. By the solar-blind UV head-mounted displays, a real-time, isometric and visible image of the corona discharge is correctly displayed upon the background scene where it exists. The user will see the visible image of the corona discharge on the real scene rather than on a small screen. Then the user can easily find out the power equipment flaws and repair them. Compared with the traditional UV imaging detector, the introducing of the HMDs simplifies the structure of the whole system. The original visible spectrum optical system is replaced by the eye in the solar-blind UV head-mounted displays. And the optical image fusion technology would be used rather than the digital image fusion system which is necessary in traditional UV imaging detector. That means the visible spectrum optical system and digital image fusion system are not necessary. This makes the whole system cheaper than the traditional UV imaging detector. Another advantage of the solar-blind UV head-mounted displays is that the two hands of user will be free. So while observing the corona discharge the user can do some things about it. Therefore the solar-blind UV head-mounted displays can make the corona discharge expose itself to the user in a better way, and it will play an important role in corona detection in the future.
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Jezová, Vera; Skládal, Jan; Eisner, Ales; Bajerová, Petra; Ventura, Karel
2007-12-07
This paper deals with comparison of efficiency of extraction techniques (solid-phase extraction, SPE and solid-phase microextraction, SPME) used for extraction of nitrate esters (ethyleneglycoldinitrate, EGDN and nitroglycerin, NG), representing the first step of the method of quantitative determination of trace concentrations of nitrate esters in water samples. EGDN and NG are subsequently determined by means of high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Optimization of SPE and SPME conditions was carried out using model water samples. Seven SPE cartridges were tested and the conditions were optimized (type of sorbent, type and volume of solvent to be used as eluent). For both nitrate esters the limit of detection (LOD) and the limit of quantification (LOQ) obtained using SPE/HPLC-UV were 0.23 microg mL(-1) and 0.70 microg mL(-1), respectively. Optimization of SPME conditions: type of SPME fibre (four fibres were tested), type and time of sorption/desorption, temperature of sorption. PDMS/DVB (polydimethylsiloxane/divinylbenzene) fibre coating proved to be suitable for extraction of EGDN and NG. For this fibre the LOD and the LOQ for both nitrate esters were 0.16 microg mL(-1) and 0.50 microg mL(-1), respectively. Optimized methods SPE/HPLC-UV and SPME/HPLC-UV were then used for quantitative determination of nitrate esters content in real water samples from the production of EGDN and NG.
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Ruzik, L; Obarski, N; Papierz, A; Mojski, M
2015-06-01
High-performance liquid chromatography (HPLC) with UV/VIS spectrophotometric detection combined with the chemometric method of cluster analysis (CA) was used for the assessment of repeatability of composition of nine types of perfumed waters. In addition, the chromatographic method of separating components of the perfume waters under analysis was subjected to an optimization procedure. The chromatograms thus obtained were used as sources of data for the chemometric method of cluster analysis (CA). The result was a classification of a set comprising 39 perfumed water samples with a similar composition at a specified level of probability (level of agglomeration). A comparison of the classification with the manufacturer's declarations reveals a good degree of consistency and demonstrates similarity between samples in different classes. A combination of the chromatographic method with cluster analysis (HPLC UV/VIS - CA) makes it possible to quickly assess the repeatability of composition of perfumed waters at selected levels of probability. © 2014 Society of Cosmetic Scientists and the Société Française de Cosmétologie.
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Aflatoxin B1 in eggs and chicken livers by dispersive liquid-liquid microextraction and HPLC.
Amirkhizi, Behzad; Arefhosseini, Seyed Rafie; Ansarin, Masoud; Nemati, Mahboob
2015-01-01
A rapid, low-cost and simple technique has been developed for the determination of aflatoxin B1 (AFB1) in eggs and livers using high-performance liquid chromatography (HPLC) with UV detection. In this study, the presence of AFB1 was investigated in 150 eggs and 50 chicken livers from the local market of Tabriz, Iran. AFB1 was extracted with a mixture of acetonitrile:water (80:20) and cleaned up by dispersive liquid-liquid microextraction which is a very economical, fast and sensitive method. AFB1 was quantified by HPLC-UV without need for any complex derivatisation in samples to enhance the detection. The results showed that 72% of the liver and 58% of the egg samples were contaminated with AFB1 ranging from 0.30 to 16.36 µg kg (̶1). limit of detection and limit of quantification for AFB1 were 0.08 and 0.28 µg kg (̶ 1), respectively. The proposed method is suitable for fast analysing of AFB1 in egg and liver samples.
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Lo Coco, F; Lanuzza, F; Micali, G; Cappellano, G
2007-01-01
Theobromine, theophylline, and caffeine are determined simultaneously by a rapid and selective reversed-phase high-performance liquid chromatography (HPLC) method with UV detection in by-products of cupuacu and cacao seeds. The determination is carried out in the raw and roasted ground cupuacu seeds and in the corresponding powders obtained after pressure treatment. The by-products of both cupuacu seeds and cacao seeds are obtained under the same technological conditions. The HPLC method uses isocratic elution with a mobile phase of methanol-water-acetic acid (80:19:1) (v/v) at a flow rate of 1 mL/min and UV absorbance detection at 275 nm. Total elution time for these analytes is less than 10 min, and the detection limit for all analytes is 0.1 mg/g. The amounts of theobromine and caffeine found in all the cupuacu samples are one or more orders of magnitude lower than those from cacao. Theophylline is found in all cacao samples except for the roasted ground paste, and it is only found in the roasted ground paste in the cupuacu samples.
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Visual Method for Detecting Contaminant on Dried Nutmeg Using Fluorescence Imaging
NASA Astrophysics Data System (ADS)
Dahlan, S. A.; Ahmad, U.; Subrata, I. D. M.
2018-05-01
Traditional practice of nutmeg sun-drying causes some fungi such as Aspergillus flavus to grow. One of the secondary metabolites of A. flavus named aflatoxin (AFs) is known to be carcinogenic, so the dried nutmeg kernel must be aflatoxin-free in the trading. Aflatoxin detection requires time and costly, make it difficult to conduct at the farmers level. This study aims to develop a simple and low-cost method to detect aflatoxin at the farmer level. Fresh nutmeg seeds were dried in two ways; sundried everyday (continuous), and sundried every two days (intermittent), both for around 18 days. The dried nutmeg seeds are then stored in a rice sack under normal conditions until the fungi grow, then they were opened and the images of kernels were captured using a CCD camera, with normal light and UV light sources. Visual observation on images captured in normal light source was able to detect the presence of fungi on dried kernels, by 28.0% for continuous and 26.2% for intermittent sun-drying. Visual observation on images captured in UV light source was able to detect the presence of aflatoxin on dried kernels, indicated by blue luminance on kernel, by 10.4% and 13.4% for continuous and intermittent sun-drying.
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Ge, Dandan; Zhang, Yi; Dai, Yixiu; Yang, Shumin
2018-04-01
Deep eutectic solvents are considered as new and green solvents that can be widely used in analytical chemistry such as microextraction. In the present work, a new dl-menthol-based hydrophobic deep eutectic solvent was synthesized and used as extraction solvents in an air-assisted dispersive liquid-liquid microextraction method for preconcentration and extraction of benzophenone-type UV filters from aqueous samples followed by high-performance liquid chromatography with diode array detection. In an experiment, the deep eutectic solvent formed by dl-menthol and decanoic acid was added to an aqueous solution containing the UV filters, and then the mixture was sucked up and injected five times by using a glass syringe, and a cloudy state was achieved. After extraction, the solution was centrifuged and the upper phase was subjected to high-performance liquid chromatography for analysis. Various parameters such as the type and volume of the deep eutectic solvent, number of pulling, and pushing cycles, solution pH and salt concentration were investigated and optimized. Under the optimum conditions, the developed method exhibited low limits of detection and limits of quantitation, good linearity, and precision. Finally, the proposed method was successfully applied to determine the benzophenone-type filters in environmental water samples with relative recoveries of 88.8-105.9%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Femtosecond UV-laser pulses to unveil protein-protein interactions in living cells.
Itri, Francesco; Monti, Daria M; Della Ventura, Bartolomeo; Vinciguerra, Roberto; Chino, Marco; Gesuele, Felice; Lombardi, Angelina; Velotta, Raffaele; Altucci, Carlo; Birolo, Leila; Piccoli, Renata; Arciello, Angela
2016-02-01
A hallmark to decipher bioprocesses is to characterize protein-protein interactions in living cells. To do this, the development of innovative methodologies, which do not alter proteins and their natural environment, is particularly needed. Here, we report a method (LUCK, Laser UV Cross-linKing) to in vivo cross-link proteins by UV-laser irradiation of living cells. Upon irradiation of HeLa cells under controlled conditions, cross-linked products of glyceraldehyde-3-phosphate dehydrogenase (GAPDH) were detected, whose yield was found to be a linear function of the total irradiation energy. We demonstrated that stable dimers of GAPDH were formed through intersubunit cross-linking, as also observed when the pure protein was irradiated by UV-laser in vitro. We proposed a defined patch of aromatic residues located at the enzyme subunit interface as the cross-linking sites involved in dimer formation. Hence, by this technique, UV-laser is able to photofix protein surfaces that come in direct contact. Due to the ultra-short time scale of UV-laser-induced cross-linking, this technique could be extended to weld even transient protein interactions in their native context.
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Apel, Christina; Tang, Jianhui; Ebinghaus, Ralf
2018-04-01
Organic UV stabilizers and UV filters are applied to industrial materials and cosmetics worldwide. In plastics they prevent photo-induced degradation, while in cosmetics they protect human skin against harmful effects of UV radiation. This study reports on the occurrence and distribution of organic UV stabilizers and UV filters in the surface sediment of the Chinese Bohai and Yellow Seas for the first time. In total, 16 out of 21 analyzed substances were positively detected. Concentrations ranged from sub-ng/g dw to low ng/g dw. The highest concentration of 25 ng/g dw was found for octocrylene (OC) in the Laizhou Bay. In the study area, characteristic composition profiles could be identified. In Korea Bay, the dominating substances were OC and ethylhexyl salicylate (EHS). All other analytes were below their method quantification limit (MQL). Around the Shandong Peninsula, highest concentrations of benzotriazole derivatives were observed in this study with octrizole (UV-329) as the predominant compound, reaching concentrations of 6.09 ng/g dw. The distribution pattern of UV-329 and bumetrizole (UV-326) were related (Pearson correlation coefficient r > 0.98, p « 0.01 around the Shandong Peninsula), indicating an identical input pathway and similar environmental behavior. Copyright © 2017 Elsevier Ltd. All rights reserved.
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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.
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Toxicity and genotoxicity of hospital laundry wastewaters treated with photocatalytic ozonation.
Kern, Deivid I; Schwaickhardt, Rômulo de O; Mohr, Geane; Lobo, Eduardo A; Kist, Lourdes T; Machado, Ênio L
2013-01-15
The aim of the present study was to assess the efficiency of advanced oxidative processes based on photocatalytic ozonation (O(3), UV, UV/O(3), UV/O(3)/Fe(2+) 50 mg L(-1) and 150 mg L(-1)) in the treatment of hospital laundry wastewaters. The analysis of the investigated wastewater revealed high chemical oxygen demand (COD - 3343.8 mg L(-1)), biochemical oxygen demand (BOD(5) - 1906.4 mg L(-1)), total Kjeldahl nitrogen (TKN - 79.8 mg L(-1)) and Daphnia magna toxicity (EC50=1.73). Genotoxic effects were also detected for Allium cepa. Reductions of some parameters occurred after photocatalytic ozonation. The UV/O(3)/Fe(2+) 150 mg L(-1) method was more efficient in reducing COD (59.1%), BOD(5) (50.3%) and TKN (86.8%). There was significant reduction (p<0.05) in D. magna toxicity, O(3) (EC50=47.3%), UV (EC50=50.6%) and UV/O(3)/Fe(2+) 150 mg L(-1) (EC50=45.4%) processes. Normalization of the mitotic index and reduction of micronucleated cells were observed in A. cepa after the treatments. Results demonstrate that these methods were efficient in the degradation of hospital laundry wastewaters, representing a thriving alternative for the removal of pollutants that cause toxicity and genotoxicity. Copyright © 2012 Elsevier B.V. All rights reserved.
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Song, Inho; Lee, Seung-Chul; Shang, Xiaobo; Ahn, Jaeyong; Jung, Hoon-Joo; Jeong, Chan-Uk; Kim, Sang-Wook; Yoon, Woojin; Yun, Hoseop; Kwon, O-Pil; Oh, Joon Hak
2018-04-11
This study investigates the performance of single-crystalline nanomaterials of wide-band gap naphthalene diimide (NDI) derivatives with methylene-bridged aromatic side chains. Such materials are found to be easily used as high-performance, visible-blind near-UV light detectors. NDI single-crystalline nanoribbons are assembled using a simple solution-based process (without solvent-inclusion problems), which is then applied to organic phototransistors (OPTs). Such OPTs exhibit excellent n-channel transistor characteristics, including an average electron mobility of 1.7 cm 2 V -1 s -1 , sensitive UV detection properties with a detection limit of ∼1 μW cm -2 , millisecond-level responses, and detectivity as high as 10 15 Jones, demonstrating the highly sensitive organic visible-blind UV detectors. The high performance of our OPTs originates from the large face-to-face π-π stacking area between the NDI semiconducting cores, which is facilitated by methylene-bridged aromatic side chains. Interestingly, NDI-based nanoribbon OPTs exhibit a distinct visible-blind near-UV detection with an identical detection limit, even under intense visible light illumination (for example, 10 4 times higher intensity than UV light intensity). Our findings demonstrate that wide-band gap NDI-based nanomaterials are highly promising for developing high-performance visible-blind UV photodetectors. Such photodetectors could potentially be used for various applications including environmental and health-monitoring systems.
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Characterizing mid-ultraviolet to optical light curves of nearby type IIn supernovae
de la Rosa, Janie; Roming, Pete; Pritchard, Tyler; ...
2016-03-21
Here, we present early mid-ultraviolet and optical observations of Type IIn supernovae (SNe IIn) observed from 2007 to 2013. Our results focus on the properties of UV light curves: peak absolute magnitudes, temporal decay, and color evolution. During early times, this sample demonstrates that UV light decays faster than optical, and each event transitions from a predominantly UV-bright phase to an optically bright phase. In order to understand early UV behavior, we generate and analyze the sample's blackbody luminosity, temperature, and radius as the SN ejecta expand and cool. Since most of our observations were detected post maximum luminosity, wemore » introduce a method for estimating the date of peak magnitude. When our observations are compared based on filter, we find that even though these SNe IIn vary in peak magnitudes, there are similarities in UV decay rates. We use a simple semi-analytical SN model in order to understand the effects of the explosion environment on our UV observations. Understanding the UV characteristics of nearby SNe IIn during an early phase can provide valuable information about the environment surrounding these explosions, leading us to evaluating the diversity of observational properties in this subclass.« less
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Dobaradaran, Sina; Lutze, Holger; Mahvi, Amir Hossein; Schmidt, Torsten C
2014-01-08
Trichloroethene and tetrachloroethene are the most common pollutants in groundwater and two of the priority pollutants listed by the U.S. Environmental Protection Agency. In previous studies on TCE and PCE photolysis and photochemical degradation, concentration ranges exceeding environmental levels by far with millimolar concentrations of TCE and PCE have been used, and it is not clear if the obtained results can be used to explain the degradation of these contaminants at more realistic environmental concentration levels. Experiments with micromolar concentrations of TCE and PCE in aqueous solution using direct photolysis and UV/H2O2 have been conducted and product formation as well as transformation efficiency have been investigated. SPME/GC/MS, HPLC/UV and ion chromatography with conductivity detection have been used to determine intermediates of degradation. The results showed that chloride was a major end product in both TCE and PCE photodegradation. Several intermediates such as formic acid, dichloroacetic acid, dichloroacetaldehyede, chloroform, formaldehyde and glyoxylic acid were formed during both, UV and UV/H2O2 treatment of TCE. However chloroacetaldehyde and chloroacetic acid were only detected during direct UV photolysis of TCE and oxalic acid was only formed during the UV/H2O2 process. For PCE photodegradation, formic acid, di- and trichloroacetic acids were detected in both UV and UV/H2O2 systems, but formaldehyde and glyoxylic acid were only detected during direct UV photolysis. For water treatment UV/H2O2 seems to be favorable over direct UV photolysis because of its higher degradation efficiency and lower risk for the formation of harmful intermediates.
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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.
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Hu, Chaofan; Jia, Li; Liu, Qingqing; Zhang, Sheng
2010-07-01
A sensitive, fast and simple method based on magnetic octadecylsilane particles was developed for the extraction of three fat-soluble vitamins followed by capillary LC (CLC) analysis with UV detection. Magnetic octadecylsilane particles were prepared based on three-step reactions including co-precipitation, sol-gel polymerization and alkylation. The characterization of the prepared product was studied by scanning electron microscope and Fourier-transform infrared spectrometry. The particles were used as magnetic SPE adsorbent for the extraction of fat-soluble vitamins in fruit juice-milk beverage. The extraction condition and efficiency of the particles for fat-soluble vitamins were investigated. By coupling magnetic SPE with capillary LC with UV detection, low concentrations of fat-soluble vitamins in fruit juice-milk beverage can be detected without the interference from other substances in the sample matrix.
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Eissa, Maya S; Abd El-Sattar, Osama I
2017-04-01
Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
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Li, Mengkai; Wang, Chen; Yau, Miaoling; Bolton, James R; Qiang, Zhimin
2017-01-01
A mini-fluidic VUV/UV photoreaction system (MVPS) was developed in our previous study, and it was demonstrated as a powerful tool for studies on pollutant degradation by the VUV/UV process. In this study, we investigated the VUV/UV photodegradation of sulfamethazine (SMN), one of the most frequently detected antibiotics in the environment. The determination methods of photochemical kinetic parameters (e.g., photon fluence-based rate constant and quantum yield) were developed based on the MVPS. The photon fluence-based reaction rate constants for SMN degradation by UV alone and VUV/UV processes were determined as 0.07 × 10 3 and 4.11 × 10 3 m 2 einstein -1 , respectively, while their quantum yields were calculated as 0.019 and 0.369, respectively. The second-order reaction rate constant between hydroxyl radical (HO • ) and SMN was determined to be 8.9 × 10 9 M -1 s -1 in VUV/UV irradiation experiments, which were conducted without addition of any other chemical. The pH effect on the SMN degradation by the VUV/UV process arose principally from SMN and HO speciation. In addition, six byproducts were identified and the potential degradation pathways of SMN including hydroxylation and SO 2 elimination were proposed. The antibacterial activity of the SMN solution, assessed by the growth inhibition tests of Escherichia coli, decreased by about 80% after VUV/UV treatment up to a photon fluence of 3.58 × 10 -3 einstein m -2 . This study has developed methods for the determination of photochemical kinetic parameters using the newly developed MVPS and has demonstrated that the VUV/UV process is an effective technology to remove sulfonamide antibiotics in water. Copyright © 2016 Elsevier Ltd. All rights reserved.
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Advances in analytical methods and occurrence of organic UV-filters in the environment--A review.
Ramos, Sara; Homem, Vera; Alves, Arminda; Santos, Lúcia
2015-09-01
UV-filters are a group of compounds designed mainly to protect skin against UVA and UVB radiation, but they are also included in plastics, furniture, etc., to protect products from light damage. Their massive use in sunscreens for skin protection has been increasing due to the awareness of the chronic and acute effects of UV radiation. Some organic UV-filters have raised significant concerns in the past few years for their continuous usage, persistent input and potential threat to ecological environment and human health. UV-filters end up in wastewater and because wastewater treatment plants are not efficient in removing them, lipophilic compounds tend to sorb onto sludge and hydrophilics end up in river water, contaminating the existing biota. To better understand the risk associated with UV-filters in the environment a thorough review regarding their physicochemical properties, toxicity and environmental degradation, analytical methods and their occurrence was conducted. Higher UV-filter concentrations were found in rivers, reaching 0.3mg/L for the most studied family, the benzophenone derivatives. Concentrations in the ng to μg/L range were also detected for the p-aminobenzoic acid, cinnamate, crylene and benzoyl methane derivatives in lake and sea water. Although at lower levels (few ng/L), UV-filters were also found in tap and groundwater. Swimming pool water is also a sink for UV-filters and its chlorine by-products, at the μg/L range, highlighting the benzophenone and benzimidazole derivatives. Soils and sediments are not frequently studied, but concentrations in the μg/L range have already been found especially for the benzophenone and crylene derivatives. Aquatic biota is frequently studied and UV-filters are found in the ng/g-dw range with higher values for fish and mussels. It has been concluded that more information regarding UV-filter degradation studies both in water and sediments is necessary and environmental occurrences should be monitored more frequently and deeply. Copyright © 2015 Elsevier B.V. All rights reserved.
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Sodium benzoate and potassium sorbate preservatives in Iranian doogh.
Zamani Mazdeh, F; Esmaeili Aftabdari, F; Moradi-Khatoonabadi, Z; Shaneshin, M; Torabi, P; Shams Ardekani, M R; Hajimahmoodi, M
2014-01-01
Sodium benzoate and potassium sorbate are two common preservatives used in Iran, yet use of these preservatives in doogh (Iranian dairy-based drink) is forbidden according to national standards. The aim of this study was to consider the presence of these preservatives in doogh by high-performance liquid chromatography with UV detection (HPLC-UV). The method was performed using a C18 column and detection at 225 nm. The mobile phase contained ammonium acetate buffer (pH = 4.2) and acetonitrile (80:20 v/v). The survey included 130 samples of doogh for identification and quantification of the named preservatives. All samples contained sodium benzoate, but potassium sorbate was detected in only 13% of them. The means of benzoate and sorbate were 21.3 ± 2.7 and 13.3 ± 39.6 mg kg(-1), respectively. The limits of detection were 2 and 40 ng g(-1) for benzoate and sorbate, respectively. Results indicate that sodium benzoate may occur in doogh naturally.
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Wang, Ji-Yu; Wang, Xin-Jie; Hui, Xian; Hua, Shui-Hong; Li, Heng; Gao, Wen-Yun
2017-03-29
Diacetyl is an important flavoring compound in many foods, especially in beer. In the present study, we developed and validated a new precolumn derivatization HPLC-UV method for the determination of diacetyl using 4-(2,3-dimethyl-6-quinoxalinyl)-1,2-benzenediamine as a novel derivatizing reagent. After derivatization with the reagent at a pH value 4.0 at ambient temperature for 10 min, diacetyl was analyzed on an ODS column and detected at 254 nm. The results show that the correlation coefficient of the method is 0.9991 in the range of 0.10 to 100.0 μM diacetyl, and the limit of detection is 0.02 μM. The method was further evaluated in the analysis of beer samples with the recoveries ranging from 94.4 to 102.6% and RSDs from 1.36 to 3.33%. The concentrations of diacetyl in 8 beer samples were determined in the range of 0.19 to 0.42 μM. The method established in this study may be well suitable for the determination of diacetyl in beer.
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Quantitative Detection of Combustion Species using Ultra-Violet Diode Lasers
NASA Technical Reports Server (NTRS)
Pilgrim, J. S.; Peterson, K. A.
2001-01-01
Southwest Sciences is developing a new microgravity combustion diagnostic based on UV diode lasers. The instrument will allow absolute concentration measurements of combustion species on a variety of microgravity combustion platforms including the Space Station. Our approach uses newly available room temperature UV diode lasers, thereby keeping the instrument compact, rugged and energy efficient. The feasibility of the technique was demonstrated by measurement of CH radicals in laboratory flames. Further progress in fabrication technology of UV diode lasers at shorter wavelengths and higher power will result in detection of transient species in the deeper UV. High sensitivity detection of combustion radicals is provided with wavelength modulation absorption spectroscopy.
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Ganareal, Thenor Aristotile Charles S; Balbin, Michelle M; Monserate, Juvy J; Salazar, Joel R; Mingala, Claro N
2018-02-12
Gold nanoparticle (AuNP) is considered to be the most stable metal nanoparticle having the ability to be functionalized with biomolecules. Recently, AuNP-based DNA detection methods captured the interest of researchers worldwide. Paratuberculosis or Johne's disease, a chronic gastroenteritis in ruminants caused by Mycobacterium avium subsp. paratuberculosis (MAP), was found to have negative effect in the livestock industry. In this study, AuNP-based probes were evaluated for the specific and sensitive detection of MAP DNA. AuNP-based probe was produced by functionalization of AuNPs with thiol-modified oligonucleotide and was confirmed by Fourier-Transform Infrared (FTIR) spectroscopy. UV-Vis spectroscopy and Scanning Electron Microscopy (SEM) were used to characterize AuNPs. DNA detection was done by hybridization of 10 μL of DNA with 5 μL of probe at 63 °C for 10 min and addition of 3 μL salt solution. The method was specific to MAP with detection limit of 103 ng. UV-Vis and SEM showed dispersion and aggregation of the AuNPs for the positive and negative results, respectively, with no observed particle growth. This study therefore reports an AuNP-based probes which can be used for the specific and sensitive detection of MAP DNA. Copyright © 2018 Elsevier Inc. All rights reserved.
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Tian, Jingzhi; Rustum, Abu
2018-02-01
Imidacloprid is used as an active pharmaceutical ingredient (API) in veterinary drugs to control fleas and ticks for dogs and cats. Here we are reporting for the first time a validated stability-indicating reversed-phase UPLC-UV method for the assay of imidacloprid and estimation of its related compounds. The stability-indicating capability of this method has been demonstrated by a forced degradation study. All related compounds including processing impurities, imidacloprid API and degradates from stressed samples were well separated from each other. Structures of major degradates from forced degradation study were elucidated through UPLC-MS/MS and key degradation pathways were proposed from the proposed chemical structures of major degradates. The UPLC-UV method is carried out using an HSS T3 column (C18, 2.1 × 30 mm, 1.8 μm particle size) maintained at 30°C with mobile phase A (0.05% v/v of phosphoric acid in water) and mobile phase B (methanol/acetonitrile 75/25 v/v). Analytes are separated by a gradient elution and detected at 270 nm. The UPLC method is green and fast with only 6.5 min run time and about 3.5 ml mobile phase consumption for each sample analysis. The UPLC-UV method was validated according to ICH guidelines. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
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Citartan, Marimuthu; Gopinath, Subash C B; Tominaga, Junji; Chen, Yeng; Tang, Thean-Hock
2014-08-01
Label-free-based detection is pivotal for real-time monitoring of biomolecular interactions and to eliminate the need for labeling with tags that can occupy important binding sites of biomolecules. One simplest form of label-free-based detection is ultraviolet-visible-near-infrared (UV-vis-NIR) spectroscopy, which measure changes in reflectivity as a means to monitor immobilization and interaction of biomolecules with their corresponding partners. In biosensor development, the platform used for the biomolecular interaction should be suitable for different molecular recognition elements. In this study, gold (Au)-coated polycarbonate was used as a platform and as a proof-of-concept, erythropoietin (EPO), a doping substance widely abused by the athletes was used as the target. The interaction of EPO with its corresponding molecular recognition elements (anti-EPO monoclonal antibody and anti-EPO DNA aptamer) is monitored by UV-vis-NIR spectroscopy. Prior to this, to show that UV-vis-NIR spectroscopy is a suitable method for measuring biomolecular interaction, the interaction between biotin and streptavidin was demonstrated via this strategy and reflectivity of this interaction decreased by 25%. Subsequent to this, interaction of the EPO with anti-EPO monoclonal antibody and anti-EPO DNA aptamer resulted in the decrease of reflectivity by 5% and 10%, respectively. The results indicated that Au-coated polycarbonate could be an ideal biosensor platform for monitoring biomolecular interactions using UV-vis-NIR spectroscopy. A smaller version of the Au-coated polycarbonate substrates can be derived from the recent set-up, to be applied towards detecting EPO abuse among atheletes. Copyright © 2014 Elsevier B.V. All rights reserved.
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Quality assessment of solar UV irradiance measured with array spectroradiometers
NASA Astrophysics Data System (ADS)
Egli, Luca; Gröbner, Julian; Hülsen, Gregor; Bachmann, Luciano; Blumthaler, Mario; Dubard, Jimmy; Khazova, Marina; Kift, Richard; Hoogendijk, Kees; Serrano, Antonio; Smedley, Andrew; Vilaplana, José-Manuel
2016-04-01
The reliable quantification of ultraviolet (UV) radiation at the earth's surface requires accurate measurements of spectral global solar UV irradiance in order to determine the UV exposure to human skin and to understand long-term trends in this parameter. Array spectroradiometers (ASRMs) are small, light, robust and cost-effective instruments, and are increasingly used for spectral irradiance measurements. Within the European EMRP ENV03 project "Solar UV", new devices, guidelines and characterization methods have been developed to improve solar UV measurements with ASRMs, and support to the end user community has been provided. In order to assess the quality of 14 end user ASRMs, a solar UV intercomparison was held on the measurement platform of the World Radiation Center (PMOD/WRC) in Davos, Switzerland, from 10 to 17 July 2014. The results of the blind intercomparison revealed that ASRMs, currently used for solar UV measurements, show a large variation in the quality of their solar UV measurements. Most of the instruments overestimate the erythema-weighted UV index - in particular at large solar zenith angles - due to stray light contribution in the UV-B range. The spectral analysis of global solar UV irradiance further supported the finding that the uncertainties in the UV-B range are very large due to stray light contribution in this wavelength range. In summary, the UV index may be detected by some commercially available ASRMs within 5 % compared to the world reference spectroradiometer, if well characterized and calibrated, but only for a limited range of solar zenith angles. Generally, the tested instruments are not yet suitable for solar UV measurements for the entire range between 290 and 400 nm under all atmospheric conditions.
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Quality assessment of solar UV irradiance measured with array spectroradiometers
NASA Astrophysics Data System (ADS)
Egli, L.; Gröbner, J.; Hülsen, G.; Bachmann, L.; Blumthaler, M.; Dubard, J.; Khazova, M.; Kift, R.; Hoogendijk, K.; Serrano, A.; Smedley, A. R. D.; Vilaplana, J.-M.
2015-12-01
The reliable quantification of ultraviolet (UV) radiation at the Earth's surface requires accurate measurements of spectral global solar UV irradiance in order to determine the UV exposure to human skin and to understand long-term trends in this parameter. Array spectroradiometers are small, light, robust and cost effective instruments and are increasingly used for spectral irradiance measurements. Within the European EMRP-ENV03 project "Solar UV", new devices, guidelines, and characterization methods have been developed to improve solar UV measurements with array spectroradiometers and support to the end-user community has been provided. In order to assess the quality of 14 end-user array spectroradiometers, a solar UV intercomparison was held on the measurement platform of the World Radiation Center (PMOD/WRC) in Davos, Switzerland, from 10 to 17 July 2014. The results of the intercomparison revealed that array spectroradiometers, currently used for solar UV measurements, show a large variation in the quality of their solar UV measurements. Most of the instruments overestimate the erythema weighted UV index - in particular at low solar zenith angles - due to stray light contribution in the UV-B range. The spectral analysis of global solar UV irradiance further supported the finding that the uncertainties in the UV-B range are very large due to stray light contribution in this wavelength range. In summary, the UV index may be detected by some commercially available array spectroradiometer within 5 % compared to the world reference spectroradiometer, if well characterized and calibrated, but only for a limited range or solar zenith angle. Generally, the tested instruments are not yet suitable for solar UV measurements for the entire range between 290 to 400 nm under all atmospheric conditions.
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UV-SPR biosensor for biomolecular interaction studies
NASA Astrophysics Data System (ADS)
Geiss, F. A.; Fossati, S.; Khan, I.; Gisbert Quilis, N.; Knoll, W.; Dostalek, J.
2017-05-01
UV surface plasmon resonance (SPR) for direct in situ detection of protein binding events is reported. A crossed relief aluminum grating was employed for diffraction coupling to surface plasmons as an alternative to more commonly used attenuated total reflection method. Wavelength interrogation of SPR was carried out by using transmission measurements in order to probe odorant-binding protein 14 (OBP14) of the honey bee (Apis mellifera). The native oxide layer on the top of an aluminum grating sensor chip allows for covalent coupling of protein molecules by using regular silane-based linkers. The probing of bound OBP14 protein at UV with confined field of surface plasmons holds potential for further studies of interaction with recently developed artificial fluorescent odorants.
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SEPARATION AND DETECTION OF THREE ARYLTINS BY CAPILLARY ELECTROPHORESIS-UV/VIS DIODE ARRAY
The trialkyltins and triphenyltins have widespread application as fungicides, antifouling coatings for porous surfaces, herbicides, insecticides, and generic biocides. Due to the varied toxicity of each species of organotins, it is important that methods address the speciation of...
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DETERMINATION OF AROMATIC AMINES IN SOILS
A rapid liquid chromatographic(LC)method with ultraviolet(UV)or fluorescence detection was developed for parts-per-billion levels of aromatic amines in soils. 2,4-Diaminotoluene, pyridine,aniline,2-picoline,2-toluidine,5-nitro-2-toluidine,2-methyl-6-ethylaniline,4-aminobiphenyl,4...
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Karimi, A.R.
In this study a method for the measurement of uranium in natural waters at sub-ppB concentration levels by the separation and determination of U/sup 4 +/ and UO/sub 2//sup 2 +/ species is proposed. Reversed phase high performance liquid chromatography, followed by a post-column reaction and a sensitive UV-visible detection system was the method of choice to determine qualitatively and quantitatively the two uranium species. Also a cation-exchange and fluorescence detection system was studied for separation and determination of UO/sub 2//sup 2 +/ ions. Uranyl ion was selectively complexed with L-phenylalanine moetie in the sample solution containing U/sup 4 +/more » ions. Uranium (IV)/U(VI)-ligand was separated on a C/sub 18/ column with acetate buffer. Hexanesulfonate was found to be the choice for ion-pair reagent. The separation was best done with the acetate buffer at .01 M concentration and pH of 3.5. Absorption of the two species were measured after a post-column reaction with Arsenazo-III. Chromatographic parameters were calculated and a calibration curves were constructed. The detection limit for the procedure was 0.7 ..mu..g/mo and 1.2..mu..g/ml for U(IV) and U(VI) respectively. When U(VI) was separated on the cation-exchange column the limit of detection was calculated to be 1 ..mu..g/ml. The direct fluorometric method for U(VI) measurement results in a detection limit of 2 ppB and upper concentration limit of 2 ppM. The effect of interfering ions in the direct method of determination could be eliminated by dilution of sample solution.« less
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A Low-Cost Liquid-Chromatography System Using a Spectronic 20-Based Detector.
ERIC Educational Resources Information Center
Jezorek, John R.; And Others
1986-01-01
Describes the design and evaluation of a Spectronic 20-based detector as well as a simple system for postcolumn derivatization useful for metal-ion chromatographic detection. Both detection and derivatization can be performed in the ultra-violet (UV) mode using a low-cost UV-visible spectrophotometer and UV-region derivatization reagents. (JN)
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Laube, Hendrik; Boden, Jana; Schneider, Roland
2017-07-01
During the production of bio-based bulk chemicals, such as lactic acid (LA), organic impurities have to be removed to produce a ready-to-market product. A capillary electrophoresis method for the simultaneous detection of LA and organic impurities in less than 10 min was developed. LA and organic impurities were detected using a direct UV detection method with micellar background electrolyte, which consisted of borate and sodium dodecyl sulfate. We investigated the effects of electrolyte composition and temperature on the speed, sensitivity, and robustness of the separation. A few validation parameters, such as linearity, limit of detection, and internal and external standards, were evaluated under optimized conditions. The method was applied for the detection of LA and organic impurities, including tyrosine, phenylalanine, and pyroglutamic acid, in samples from a continuous LA fermentation process from post-extraction tapioca starch and yeast extract.
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NASA Astrophysics Data System (ADS)
Shkolyar, S.; Eshelman, E.; Farmer, J. D.; Hamilton, D.; Daly, M. G.; Youngbull, C.
2017-12-01
The Mars 2020 mission will analyze samples in situ and identify any that could have preserved biosignatures in ancient habitable environments for later return to Earth. Highest-priority targeted samples include aqueously formed sedimentary lithologies containing fossil biosignatures as aromatic carbon (kerogen). In this study, we analyze non-extracted, naturally preserved kerogen in a diverse suite of realistic Mars analogs using combined UV excitation time-gated (UV-TG) Raman and laser-induced fluorescence spectroscopy. We interrogated kerogen and its host matrix in samples to: (1) explore the capabilities of UV-TG Raman and fluorescence spectroscopy for detecting kerogen in high-priority targets in the search for a Martian fossil record; (2) assess the effectiveness of time-gating and UV laser wavelength in reducing fluorescence; and (3) identify sample-specific issues which could challenge rover-based identifications of kerogen using UV-TG Raman spectroscopy. We found that ungated UV Raman is suited to identify diagnostic kerogen Raman bands without interfering fluorescence and that fluorescence features indicating kerogen are detectable. These data highlight the value of using both co-located Raman and fluorescence data sets together to strengthen the confidence of kerogen detection as a potential biosignature and are obtainable by SHERLOC onboard Mars 2020.
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Identification of forensic samples by using an infrared-based automatic DNA sequencer.
Ricci, Ugo; Sani, Ilaria; Klintschar, Michael; Cerri, Nicoletta; De Ferrari, Francesco; Giovannucci Uzielli, Maria Luisa
2003-06-01
We have recently introduced a new protocol for analyzing all core loci of the Federal Bureau of Investigation's (FBI) Combined DNA Index System (CODIS) with an infrared (IR) automatic DNA sequencer (LI-COR 4200). The amplicons were labeled with forward oligonucleotide primers, covalently linked to a new infrared fluorescent molecule (IRDye 800). The alleles were displayed as familiar autoradiogram-like images with real-time detection. This protocol was employed for paternity testing, population studies, and identification of degraded forensic samples. We extensively analyzed some simulated forensic samples and mixed stains (blood, semen, saliva, bones, and fixed archival embedded tissues), comparing the results with donor samples. Sensitivity studies were also performed for the four multiplex systems. Our results show the efficiency, reliability, and accuracy of the IR system for the analysis of forensic samples. We also compared the efficiency of the multiplex protocol with ultraviolet (UV) technology. Paternity tests, undegraded DNA samples, and real forensic samples were analyzed with this approach based on IR technology and with UV-based automatic sequencers in combination with commercially-available kits. The comparability of the results with the widespread UV methods suggests that it is possible to exchange data between laboratories using the same core group of markers but different primer sets and detection methods.
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He, Yongzhen; Dai, Chaomeng; Zhou, Xuefei
2017-01-01
A magnetic spinel cobalt ferrite nanoparticle composite (CFO) was prepared via an ultrasonication-assisted co-precipitation method. The morphological structure and surface composition of CFO before and after reaction were investigated by using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray, and Fourier transform infrared spectroscopy, indicating the consumption of iron oxide during photodegradation. X-ray photoelectron spectroscopy and vibrating sample magnetometry confirm the preparation of the ferrite nanoparticle composite and its magnetic properties. The prepared CFO was then used for the photocatalytic degradation of carbamazepine (CBZ) as an example of pharmaceuticals and personal care products (PPCPs) from aqueous solution. The effects of the nanocomposite dosage, contact time, and solution pH on the photodegradation process were investigated. More than 96% of the CBZ was degraded within 100 min at 0.2 g·L -1 CFO in the presence of UV light. The reactive species for CBZ degradation in the CFO/UV system was identified as hydroxyl radicals by the methanol scavenging method. Combined with the detection of leached iron ions during the process, the CBZ degradation mechanism can be presumed to be heterogeneous and homogeneous photocatalytic degradation in the CFO/UV system. Furthermore, iminostilbene and acridine were detected as intermediate products by GC-MS.
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Aresta, Antonella; Cioffi, Nicola; Palmisano, Francesco; Zambonin, Carlo G
2003-08-27
A solid-phase microextraction (SPME) method, coupled to liquid chromatography with diode array UV detection (LC-UV/DAD), for the simultaneous determination of cyclopiazonic acid, mycophenolic acid, tenuazonic acid, and ochratoxin A is described. Chromatographic separation was achieved on a propylamino-bonded silica gel stationary phase using acetonitrile/methanol/ammonium acetate buffer mixture (78:2:20, v/v/v) as mobile phase. SPME adsorption and desorption conditions were optimized using a silica fiber coated with a 60 microm thick polydimethylsiloxane/divinylbenzene film. Estimated limits of detection and limits of quantitation ranged from 3 to 12 ng/mL and from 7 to 29 ng/mL, respectively. The method has been applied to cornflake samples. Samples were subjected to a preliminary short sonication in MeOH/2% KHCO(3) (70:30, v/v); the mixture was evaporated to near dryness and reconstituted in 1.5 mL of 5 mM phosphate buffer (pH 3) for SPME followed by LC-UV/DAD. The overall procedure had recoveries (evaluated on samples spiked at 200 ng/g level) ranging from 74 +/- 4 to 103 +/- 9%. Samples naturally contaminated with cyclopiazonic and tenuazonic acids were found; estimated concentrations were 72 +/- 9 and 25 +/- 6 ng/g, respectively.
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[Early warning for various internal faults of GIS based on ultraviolet spectroscopy].
Zhao, Yu; Wang, Xian-pei; Hu, Hong-hong; Dai, Dang-dang; Long, Jia-chuan; Tian, Meng; Zhu, Guo-wei; Huang, Yun-guang
2015-02-01
As the basis of accurate diagnosis, fault early-warning of gas insulation switchgear (GIS) focuses on the time-effectiveness and the applicability. It would be significant to research the method of unified early-warning for partial discharge (PD) and overheated faults in GIS. In the present paper, SO2 is proposed as the common and typical by-product. The unified monitoring could be achieved through ultraviolet spectroscopy (UV) detection of SO2. The derivative method and Savitzky-Golay filtering are employed for baseline correction and smoothing. The wavelength range of 290-310 nm is selected for quantitative detection of SO2. Through UV method, the spectral interference of SF6 and other complex by-products, e.g., SOF2 and SOF2, can be avoided and the features of trace SO2 in GIS can be extracted. The detection system is featured by compacted structure, low maintenance and satisfactory suitability in filed surveillance. By conducting SF6 decomposition experiments, including two types of PD faults and the overheated faults between 200-400 degrees C, the feasibility of proposed UV method has been verified. Fourier transform infrared spectroscopy and gas chromatography methods can be used for subsequent fault diagnosis. The different decomposition features in two kinds of faults are confirmed and the diagnosis strategy has been briefly analyzed. The main by-products under PD are SOF2 and SO2F2. The generated SO2 is significantly less than SOF2. More carbonous by-products will be generated when PD involves epoxy. By contrast, when the material of heater is stainless steel, SF6 decomposes at about 300 "C and the main by-products in overheated faults are SO2 and SO2F2. When heated over 350 degrees C, SO2 is generated much faster. SOz content stably increases when the GIS fault lasts. The faults types could be preliminarily identified based on the generation features of SO2.
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The system of high accuracy UV spectral radiation system
NASA Astrophysics Data System (ADS)
Lin, Guan-yu; Yu, Lei; Xu, Dian; Cao, Dian-sheng; Yu, Yu-Xiang
2016-10-01
UV spectral radiation detecting and visible observation telescope is designed by the coaxial optical. In order to decrease due to the incident light polarization effect, and improve the detection precision, polarizer need to be used in the light path. Four pieces of quartz of high Precision UV radiation depolarizer retarder stack together is placed in front of Seya namioka dispersion unit. The coherent detection principle of modulation of light signal and the reference signal multiplied processing, increase the phase sensitive detector can be adjustment function, ensure the UV spectral radiation detection stability. A lock-in amplifier is used in the electrical system to advance the accuracy of measurement. To ensure the precision measurement detected, the phase-sensitive detector function can be adjustable. the output value is not more than 10mV before each measurement, so it can be ensured that the stability of the measured radiation spectrum is less than 1 percent.
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[Study on UPLC-UV-MS fingerprints of different medicinal parts of Poria cocos].
Li, Ke; Zhang, Li-Qun; Nie, Jing
2013-03-01
To establish an analytical method for the fingerprint of triterpenoid constituents of Poria cocos by UPLC-UV-MS and compare the fingerprints of different medicinal parts of Poria cocos. With dehydropachymic acid as reference substance, the separation was performed on Shim-pack XR-ODS II (75 mm x 2.0 mm, 2.2 microm) analytical column. The mobile phase was consisted of acetonitrile and 0.1% formic acid as gradient eluent. The UV detection wavelength was 242 nm. The flow rate was 0.5 mL/min. The column temperature was 30 degrees C. The cluster analysis was carried on by SPSS 16. 0. The UPLC-UV-MS fingerprints of triterpenoid constituents of Poria cocos were set up. The result showed that 22 peaks were found in different medicinal parts and 12 peaks of them were common. The results of method validation met technical requirement of fingerprints; Triterpenoid constituents in pared skin of Poria and peeled and sliced Poria were different, and the effect of habitat on the quality of peeled and sliced Poria was more obvious than that of pared skin of Poria. The method is stable and reliable with a good reproducibility and provides a reference standard for the quality control of Poria cocos.
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Ultraviolet Satellite Measurements of Volcanic Ash. Chapter 12
NASA Technical Reports Server (NTRS)
Carn, S. A.; Krotkov, N. A.
2016-01-01
Ultraviolet (UV) remote sensing of volcanic ash and other absorbing aerosols from space began with the launch of the first Total Ozone Mapping Spectrometer (TOMS) instrument in 1978. Subsequent UV satellite missions (TOMS, GOME, SCIAMACHY, OMI, GOME-2, OMPS) have extended UV ash measurements to the present, generating a unique multidecadal record. A UV Aerosol Index (UVAI) based on two near-UV wavelengths, equally applicable to multispectral (TOMS, DSCOVR) or hyperspectral (GOME, SCIAMACHY, OMI, GOME-2, OMPS) instruments, has been used to derive a unique absorbing aerosol climatology across multiple UV satellite missions. Advantages of UV ash measurements relative to infrared (IR) techniques include the ability to detect ash at any altitude (assuming no clouds), above clouds, and over bright surfaces, where visible and IR techniques may fail. Disadvantages include the daytime-only restriction and nonspecificity to silicate ash, since UV measurements are sensitive to any UV-absorbing aerosol, including smoke, desert dust, and pollution. However, simultaneous retrieval of sulfur dioxide (SO2) abundance and UVAI provides robust discrimination of volcanic clouds. Although the UVAI is only semiquantitative, it has proved successful at detecting and tracking volcanic ash clouds from many volcanic eruptions since 1978. NASA A-Train measurements since 2006 (eg, CALIOP) have provided much improved constraints on volcanic ash altitude, and also permit identification of aerosol type through sensor synergy. Quantitative UV retrievals of ash optical depth, effective particle size, and ash column mass are possible and require assumptions of ash refractive index, particle size distribution, and ash layer altitude. The lack of extensive ash refractive index data in the UV-visible and the effects of ash particle shape on retrievals introduce significant uncertainty in the retrieved parameters, although limited validation against IR ash retrievals has been successful. In this contribution, we review UV ash detection and retrieval techniques and provide examples of volcanic eruptions detected in the approx. 37 year data record.
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Sengupta, Partha Pratim; Gloria, Jared N; Amato, Dahlia N; Amato, Douglas V; Patton, Derek L; Murali, Beddhu; Flynt, Alex S
2015-10-12
Detection of specific RNA or DNA molecules by hybridization to "probe" nucleic acids via complementary base-pairing is a powerful method for analysis of biological systems. Here we describe a strategy for transducing hybridization events through modulating intrinsic properties of the electroconductive polymer polyaniline (PANI). When DNA-based probes electrostatically interact with PANI, its fluorescence properties are increased, a phenomenon that can be enhanced by UV irradiation. Hybridization of target nucleic acids results in dissociation of probes causing PANI fluorescence to return to basal levels. By monitoring restoration of base PANI fluorescence as little as 10(-11) M (10 pM) of target oligonucleotides could be detected within 15 min of hybridization. Detection of complementary oligos was specific, with introduction of a single mismatch failing to form a target-probe duplex that would dissociate from PANI. Furthermore, this approach is robust and is capable of detecting specific RNAs in extracts from animals. This sensor system improves on previously reported strategies by transducing highly specific probe dissociation events through intrinsic properties of a conducting polymer without the need for additional labels.
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Liquid Chromatographic Analysis of α-Dicarbonyls Using Girard-T Reagent Derivatives.
Lawrence, Glen D; Rahmat, Rozaiha; Makahleh, Ahmad; Saad, Bahruddin
2017-11-01
The measurement of α-dicarbonyls and other degradation products of sugars has become important in view of their toxicity. Although there are several methods used for their analysis, most require long reaction times to form UV absorbing or fluorescent derivatives and the nonpolar nature of commonly used derivatives necessitates relatively high concentrations of organic solvents for elution in reverse phase liquid chromatography. The present method describes the use of Girard-T reagent in a simple, one step derivatization of α-dicarbonyls and conjugated aldehydes and analysis using ion-pair reverse phase liquid chromatography. The limit of detection was in the range of 0.06-0.09 μM (4-12 ng/mL) for glyoxal, methylglyoxal, 3-deoxyglucosone and 5-hydroxymethylfurfural with good linear response and reproducibility using UV detection. The hydrazone derivatives were stable for several days in solution. The method was used to study degradation of several sugars and quantification of the target α-dicarbonyls and 5-hydroxymethylfurfural in several soft drinks. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
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Amirjani, Amirmostafa; Fatmehsari, Davoud Haghshenas
2018-01-01
In this work, a rapid and straightforward method was developed for colorimetric determination of ammonia using smartphones. The mechanisms is based on the manipulation of the surface plasmon band of silver nanoparticles (AgNPs) via the formation of Ag (NH 3 ) 2 + complex. This complex decreases the amount of AgNPs in the solution and consequently, the color intensity of the colloidal system decreases. Not only the variation in color intensity of the solution can be tracked by a UV-vis spectrophotometer, but also a smartphone can be employed to monitor the color intensity variation by RGB analysis. Ammonia, in the concentration range of 10-1000mgL -1 , was successfully measured spectrophotometrically (UV-vis spectrophotometer) and colorimetrically (RGB measurement) with the detection limit of 180 and 200mgL -1 , respectively. Linear relationships were also developed for both methods. Also, the response time of the developed colorimetric sensor was around 20s. Both of the colorimetric and spectrophotometric methods showed a reliable performance for determination of ammonia in the real samples. Copyright © 2017 Elsevier B.V. All rights reserved.
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Salem, Hesham
2010-01-01
Three methods were developed for simultaneous determination of metformin hydrochloride and glyburide in an antihyperglycemic binary mixture without previous separation. In the first method, a reversed-phase HPLC column with acetonitrile-water (60 + 40, v/v) mobile phase at 0.9 mL/min flow rate was used to separate both compounds, with UV detection at 254 nm. Linearity was obtained in the concentration range of 0.06--0.24 microg/mL for glyburide and 1.5-6.0 microg/mL for metformin hydrochloride. The second method depended on first- and second-derivative UV spectrometry with zero-crossing measurements. The first-derivative amplitude at 261 nm was selected for the assay of glyburide, and the second-derivative amplitude at 235 nm was selected for the assay of metformin hydrochloride. The third method depended on measuring the first derivative of the ratio-spectra at 241 nm for glyburide and 227 nm for metformin hydrochloride. For the second and third methods, Beer's law was obeyed in the range of 10-55 microg/mL for glyburide and 20-200 microg/mL for metformin. The proposed methods were extensively validated and applied for the analysis of some pharmaceutical formulations containing binary mixtures of the mentioned drugs.
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NASA Astrophysics Data System (ADS)
Hug, William F.; Bhartia, Rohit; Taspin, Alexandre; Lane, Arthur; Conrad, Pamela; Sijapati, Kripa; Reid, Ray D.
2005-11-01
Laser induced native fluorescence (LINF) is the most sensitive method of detection of biological material including microorganisms, virus', and cellular residues. LINF is also a sensitive method of detection for many non-biological materials as well. The specificity with which these materials can be classified depends on the excitation wavelength and the number and location of observation wavelengths. Higher levels of specificity can be obtained using Raman spectroscopy but a much lower levels of sensitivity. Raman spectroscopy has traditionally been employed in the IR to avoid fluorescence. Fluorescence rarely occurs at wavelength below about 270nm. Therefore, when excitation occurs at a wavelength below 250nm, no fluorescence background occurs within the Raman fingerprint region for biological materials. When excitation occurs within electronic resonance bands of the biological target materials, Raman signal enhancement over one million typically occurs. Raman sensitivity within several hundred times fluorescence are possible in the deep UV where most biological materials have strong absorption. Since the Raman and fluorescence emissions occur at different wavelength, both spectra can be observed simultaneously, thereby providing a sensor with unique sensitivity and specificity capability. We will present data on our integrated, deep ultraviolet, LINF/Raman instruments that are being developed for several applications including life detection on Mars as well as biochemical warfare agents on Earth. We will demonstrate the ability to discriminate organic materials based on LINF alone. Together with UV resonance Raman, higher levels of specificity will be demonstrated. In addition, these instruments are being developed as on-line chemical sensors for industrial and municipal waste streams and product quality applications.
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Tsai, Chia-Ju; Chen, Yen-Ling; Feng, Chia-Hsien
2013-10-04
This study explored dispersive liquid-liquid microextraction for extraction and concentration of lipoic acid in human urine. To improve the detection of lipoic acid by both capillary liquid chromatography (CapLC) with UV detection and matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), microwave-assisted derivatization with 4-bromomethyl-6,7-dimethoxycoumarin was performed to render lipoic acid chromophores for UV detection and also high ionization efficiency in MALDI. All parameters that affected lipoic acid extraction and derivatization from urine were investigated and optimized. In the analyses of human urine samples, the two methods had a linear range of 0.1-20 μM with a correlation coefficient of 0.999. The detection limits of CapLC-UV and MALDI-TOF MS were 0.03 and 0.02 μM (S/N ≧ 3), respectively. The major metabolites of lipoic acid, including 6,8-bismethylthio-octanoic acid, 4,6-bismethylthio-hexanoic acid, and 2,4-bismethylthio-butanoic acid were also extracted by dispersive liquid-liquid microextraction and detected by MALDI-TOF MS. The minor metabolites (undetectable by MALDI-TOF MS), bisnorlipoic acid and tetranorlipoic acid were also extracted by dispersive liquid-liquid microextraction and identified with an LTQ Orbitrap mass spectrometer. After dispersive liquid-liquid microextraction and microwave-assisted derivatization, all lipoic acid derivatizations and metabolites were structurally confirmed by LTQ Orbitrap. Copyright © 2013 Elsevier B.V. All rights reserved.
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Kanazawa, Hideko; Tsubayashi, Akane; Nagata, Yoshiko; Matsushima, Yoshikazu; Mori, Chiharu; Kizu, Junko; Higaki, Megumu
2002-03-01
The chiral separation of loxoprofen was achieved on a chiral column with UV and circular dichroism (CD) detection. The good resolution of four loxoprofen stereoisomers was obtained. The column used for the chiral separation was Chiralcel OJ column (250 x 4.6 mm) using hexane-2-propanol-trifluoroacetic acid (95:5:0.1), as an eluent. The flow-rate was 1.0 ml/min and the detection was at 225 nm. In addition, CD and UV spectra were obtained by stopped flow scanning. The method allows the determination of the stereoisomers of loxoprofen in human plasma after the administration of therapeutic dose of the racemic drug, thus HPLC with CD detector is useful for the stereospecific determination of loxoprofen products in biological samples.
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Zhao, Qi; Ding, Jie; Jin, Haiyan; Ding, Lan; Ren, Nanqi
2013-04-01
A method based on cloud point extraction (CPE) coupled with high-performance liquid chromatography separation and ultraviolet (UV) detection was developed to determine andrographolide and dehydroandrographolide in human plasma. The nonionic surfactant Triton X-114 was chosen as the extraction medium. Variable parameters affecting the CPE efficiency were evaluated and optimized, such as concentrations of Triton X-114 and NaCl, pH, equilibration temperature and equilibration time. A Zorbax SB C18 column (250 × 4.6 mm i.d., 5 µm) was used for separation of the two analytes at 30°C. The UV detection was performed at 254 nm. Under the optimum conditions, the limits of detection of andrographolide and dehydroandrographolide are 0.032 and 0.019 µg/mL, respectively. The intra-day and inter-day precisions expressed as relative standard deviation ranged from 3.2 to 7.3% and from 2.9 and 8.6%. The recoveries of andrographolide and dehydroandrographolide were in the range of 76.8-98.6% at three fortified concentrations of 0.1, 0.5 and 1.0 µg/mL. This method was efficient, environmentally friendly, rapid and inexpensive for the extraction and determination of andrographolide and dehydroandrographolide in human plasma.
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NASA Astrophysics Data System (ADS)
Loureiro, A. D.; Gomes, L. M.; Ventura, L.
2018-02-01
The international standard ISO 12312-1 proposes transmittance tests that quantify how dark sunglasses lenses are and whether or not they are suitable for driving. To perform these tests a spectrometer is required. In this study, we present and analyze theoretically an accurate alternative method for performing these measurements using simple components. Using three LEDs and a four-channel sensor we generated weighting functions similar to the standard ones for luminous and traffic lights transmittances. From 89 sunglasses lens spectroscopy data, we calculated luminous transmittance and signal detection quotients using our obtained weighting functions and the standard ones. Mean-difference Tukey plots were used to compare the results. All tested sunglasses lenses were classified in the right category and correctly as suitable or not for driving. The greatest absolute errors for luminous transmittance and red, yellow, green and blue signal detection quotients were 0.15%, 0.17, 0.06, 0.04 and 0.18, respectively. This method will be used in a device capable to perform transmittance tests (visible, traffic lights and ultraviolet (UV)) according to the standard. It is important to measure rightly luminous transmittance and relative visual attenuation quotients to report correctly whether or not sunglasses are suitable for driving. Moreover, standard UV requirements depend on luminous transmittance.
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Every year over 250 million pounds of cyanuric acid (CA) and chloroisocyanurates are produced industrially. These compounds are standard ingredients in formulations for household bleaches, industrial cleansers, dishwasher compounds, general sanitizers, and chlorine stabilizers. ...
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Purves, Randy W; Khazaei, Hamid; Vandenberg, Albert
2018-02-01
Faba bean (Vicia faba L.) provides environmental and health benefits; however, the presence of the pyrimidine glycosides vicine and convicine (v-c) in its seeds limits consumption. Low v-c genotypes have been introduced, but the convicine levels in these genotypes have not been quantified. To improve detection, the polar nature of v-c was exploited by implementing hydrophilic interaction liquid chromatography (HILIC). A sample preparation method using a two-step extraction was developed for use with UV and/or tandem mass spectrometry (SRM) detection. The HILIC-UV method was suitable for over three orders of magnitude, covering the range of v-c concentrations in faba bean seeds across all genotypes tested. The linear range of HILIC-SRM was slightly less (∼3 orders of magnitude), but improved sensitivity and selectivity make it more suitable for quantifying low v-c samples. The analysis of 13 genotypes suggests that v-c concentrations in faba bean seeds may be independent quantitative traits. Copyright © 2017 Elsevier Ltd. All rights reserved.
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Frederiksen, Hanne; Nielsen, Ole; Skakkebaek, Niels E; Juul, Anders; Andersson, Anna-Maria
2017-03-01
Experimental studies indicate that some chemicals with UV blocking properties (known as UV filters) can act as endocrine disruptors. UV filters are used in sunscreens and other cosmetic- and personal care products, as well as in other consumer products such as food packaging, clothing and furniture textiles to protect the products against UV radiation. Here we present the urinary excretion of suspected endocrine active UV filters in Danish children and adolescents recruited from the general population. The content of benzophenone (BP), benzophenone-1 (BP-1), benzophenone-2 (BP-2), benzophenone-3 (BP-3), 5-chloro-2- hydroxybenzophenone (BP-7), 4-hydroxybenzophenone (4-HBP), 4-methyl-benzophenone (4-MBP), 3-(4- methylbenzylidene)-camphor (4-MBC) and 3-benzylidene camphor (3-BC) were monitored in 24h urine and two consecutive first morning samples from 129 healthy Danish children and adolescents (6-21 yrs). All 387 samples were collected during the autumn (Nov. 2007) and were analyzed by a new on-line TurboFlow-LC-MS/MS method developed for simultaneous biomonitoring of these nine UV filters in urine. BP-3 and BP-1 were detected in more than 80% of the 24h samples and were significantly correlated (R 2 =0.815). BP, 4-HBP and BP-2 were found in 43, 15 and 5% of the samples, respectively. The median (range) concentrations of the UV-filters in 24-h urine were as follows: BP-3, 0.92 (LOD-115); BP-1, 0.54 (LOD-44.6); BP,
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Langer, Swen; Lodge, John K
2014-06-01
Water-soluble vitamins are an important class of compounds that require quantification from food sources to monitor nutritional value. In this study we have analysed six water-soluble B vitamins ([thiamine (B1), riboflavin (B2), nicotinic acid (B3, NAc), nicotinamide (B3, NAm), pyridoxal (B6), folic acid (B9)], and ascorbic acid (vit C) with hydrophilic interaction liquid chromatography (HILIC), and compared UV, fluorescent (FLD) and coulometric detection to optimise a method to quantitate the vitamins from food sources. Employing UV/diode array (DAD) and fluorimetric detection, six B vitamins were detected in a single run using gradient elution from 100% to 60% solvent B [10mM ammonium acetate, pH 5.0, in acetonitrile and water 95:5 (v:v)] over 18 min. UV detection was performed at 268 nm for B1, 260 nm for both B3 species and 284 nm for B9. FLD was employed for B2 at excitation wavelength of 268 nm, emission of 513 nm, and 284 nm/317 nm for B6. Coulometric detection can be used to detect B6 and B9, and vit C, and was performed isocratically at 75% and 85% of solvent B, respectively. B6 was analysed at a potential of 720 mV, while B9 was analysed at 600 mV, and vit C at 30 mV. Retention times (0.96 to 11.81 min), intra-day repeatability (CV 1.6 to 3.6), inter-day variability (CV 1.8 to 11.1), and linearity (R 0.9877 to 0.9995) remained good under these conditions with limits of detection varying from 6.6 to 164.6 ng mL(-1), limits of quantification between 16.8 and 548.7 ng mL(-1). The method was successfully applied for quantification of six B vitamins from a fortified food product and is, to our knowledge, the first to simultaneously determine multiple water-soluble vitamins extracted from a food matrix using HILIC. Copyright © 2014 Elsevier B.V. All rights reserved.
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Torrecilla, José S; Rojo, Ester; Domínguez, Juan C; Rodríguez, Francisco
2010-02-10
A simple and novel method to quantify adulterations of extra virgin olive oil (EVOO) with refined olive oil (ROO) and refined olive-pomace oil (ROPO) is described here. This method consists of calculating chaotic parameters (Lyapunov exponent, autocorrelation coefficients, and two fractal dimensions, CPs) from UV-vis scans of adulterated EVOO samples. These parameters have been successfully linearly correlated with the ROO or ROPO concentrations in 396 EVOO adulterated samples. By an external validation process, when the adulterating agent concentration is less than 10%, the integrated CPs/UV-vis model estimates the adulterant agent concentration with a mean correlation coefficient (estimated versus real concentration of low grade olive oil) greater than 0.97 and a mean square error of less than 1%. In light of these results, this detector is suitable not only to detect adulterations but also to measure impurities when, for instance, a higher grade olive oil is transferred to another storage tank in which lower grade olive oil was stored that had not been adequately cleaned.
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Kaddoumi, A; Kubota, A; Nakashima, M N; Takahashi, M; Nakashima, K
2001-10-01
A high performance liquid chromatographic method has been developed for the simultaneous determination of (+/-) fenfluramine (Fen) and phentermine (Phen) in addition to three other sympathomimetic amines-ephedrine (E), norephedrine (NE) and 2-phenylethylamine (2-PEA), using cyclohexylamine (CX) as an internal standard in plasma. The compounds were derivatized with 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride (DIB-Cl) to give the DIB-derivatives. The derivatives were then separated using an isocratic HPLC system with UV detection. The limits of detection for Fen, Phen, E, NE and 2-PEA in plasma ranged from 0.32 to 22.9 pmol on column at a signal-to-noise ratio of 3. The recoveries following alkaline extraction from plasma samples of known concentrations were found to be more than 94% for the studied compounds. This method might be useful for the screening of the studied sympathomimetic amines in human plasma samples in forensic as well as toxicological studies. Furthermore, the developed method was modified for the simultaneous determination of Fen and Phen in human and rat plasma using fluoxetine as an internal standard. The methods are reproducible and precise. Finally, the two drugs were administered intraperitoneally to rats in combination, and their plasma levels over the investigated time course were successfully determined. Copyright 2001 John Wiley & Sons, Ltd.
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Analysis of aromatic aldehydes in brandy and wine by high-performance capillary electrophoresis.
Panossian, A; Mamikonyan, G; Torosyan, M; Gabrielyan, E; Mkhitaryan, S
2001-09-01
A new method of analysis of vanillin, syringaldehyde, coniferaldehyde, and sinapaldehyde in brandy and wine by high-performance capillary electrophoresis is described. Electrophoretic mobility of these compounds is achieved by a borate buffer at pH 9.3. At this pH, the sensitivity of UV detection of these phenolic aldehydes also increases. UV absorptions at 348, 362, 404, and 422 nm were selected for monitoring vanillin, syringaldehyde, coniferaldehyde, and sinapaldehyde, respectively. This procedure was performed simultaneously during one run using a diode array detector. Samples of brandy or wine were analyzed directly without concentration, extraction, or any other preliminary treatment of the test sample. The limits of detection were found to be 0.275, 0.1425, 0.1475, and 0.1975 ppm for syringaldehyde, coniferaldehyde, sinapaldehyde, and vanillin, respectively, which is acceptable for analysis of both brandy and wine aged in oak barrels. The method has been shown to be linear in a range from 0.3 to 57 mg/L. Recoveries ranged between 99.9% and 107.7% for all of the compounds tested. Repeatability and reproducibility of the method were high. The relative standard deviation was consequently approximately 3% and also between 4.47% and 6.89% for all tested compounds. The method is useful for the identification of counterfeit brandy, which is easy to recognize by the absence of sinapaldehyde, syringaldehyde, and coniferaldehyde, which are not detectable in false brandy.
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Fish freshness estimation using eye image processing under white and UV lightings
NASA Astrophysics Data System (ADS)
Kanamori, Katsuhiro; Shirataki, Yuri; Liao, Qiuhong; Ogawa, Yuichi; Suzuki, Tetsuhito; Kondo, Naoshi
2017-05-01
A non-destructive method of estimating the freshness of fish is required for appropriate price setting and food safety. In particular, for determining the possibility of eating raw fish (sashimi), freshness estimation is critical. We studied such an estimation method by capturing images of fish eyes and performing image processing using the temporal changes of the luminance of pupil and iris. To detect subtle non-visible changes of these features, we used UV (375 nm) light illumination in addition to visible white light illumination. Polarization and two-channel LED techniques were used to remove strong specular reflection from the cornea of the eye and from clear-plastic wrap used to cover the fish to maintain humidity. Pupil and iris regions were automatically detected separately by image processing after the specular reflection removal process, and two types of eye contrast were defined as the ratio of mean and median pixel values of each region. Experiments using 16 Japanese dace (Tribolodon hakonensis) at 23° and 85% humidity for 24 hours were performed. The eye contrast of raw fish increase non-linearly in the initial period and then decreased; however, that of frozen-thawed fish decreased linearly throughout 24 hours, regardless of the lighting. Interestingly, the eye contrast using UV light showed a higher correlation with time than that using white light only in the case of raw fish within the early 6- hour period postmortem. These results show the possibility of estimating fish freshness in the initial stage when fish are eaten raw using white and UV lightings.
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Fischbach, Jens; Xander, Nina Carolin; Frohme, Marcus; Glökler, Jörn Felix
2015-04-01
The need for simple and effective assays for detecting nucleic acids by isothermal amplification reactions has led to a great variety of end point and real-time monitoring methods. Here we tested direct and indirect methods to visualize the amplification of potato spindle tuber viroid (PSTVd) by loop-mediated isothermal amplification (LAMP) and compared features important for one-pot in-field applications. We compared the performance of magnesium pyrophosphate, hydroxynaphthol blue (HNB), calcein, SYBR Green I, EvaGreen, and berberine. All assays could be used to distinguish between positive and negative samples in visible or UV light. Precipitation of magnesium-pyrophosphate resulted in a turbid reaction solution. The use of HNB resulted in a color change from violet to blue, whereas calcein induced a change from orange to yellow-green. We also investigated berberine as a nucleic acid-specific dye that emits a fluorescence signal under UV light after a positive LAMP reaction. It has a comparable sensitivity to SYBR Green I and EvaGreen. Based on our results, an optimal detection method can be chosen easily for isothermal real-time or end point screening applications.
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Satínský, Dalibor; Huclová, Jitka; Ferreira, Raquel L C; Montenegro, Maria Conceição B S M; Solich, Petr
2006-02-13
The porous monolithic columns show high performance at relatively low pressure. The coupling of short monoliths with sequential injection technique (SIA) results in a new approach to implementation of separation step to non-separation low-pressure method. In this contribution, a new separation method for simultaneous determination of ambroxol, methylparaben and benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith SpeedROD RP-18e, 50-4.6 mm column with 10 mm precolumn and a FIAlab 3000 system with a six-port selection valve and 5 ml syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-tetrahydrofuran-0.05M acetic acid (10:10:90, v/v/v), pH 3.75 adjusted with triethylamine, flow rate 0.48 mlmin(-1), UV-detection was at 245 nm. The analysis time was <11 min. A new SIC method was validated and compared with HPLC. The method was found to be useful for the routine analysis of the active compounds ambroxol and preservatives (methylparaben or benzoic acid) in various pharmaceutical syrups and drops.
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Popa-Burke, Ioana G; Issakova, Olga; Arroway, James D; Bernasconi, Paul; Chen, Min; Coudurier, Louis; Galasinski, Scott; Jadhav, Ajit P; Janzen, William P; Lagasca, Dennis; Liu, Darren; Lewis, Roderic S; Mohney, Robert P; Sepetov, Nikolai; Sparkman, Darren A; Hodge, C Nicholas
2004-12-15
As part of an overall systems approach to generating highly accurate screening data across large numbers of compounds and biological targets, we have developed and implemented streamlined methods for purifying and quantitating compounds at various stages of the screening process, coupled with automated "traditional" storage methods (DMSO, -20 degrees C). Specifically, all of the compounds in our druglike library are purified by LC/MS/UV and are then controlled for identity and concentration in their respective DMSO stock solutions by chemiluminescent nitrogen detection (CLND)/evaporative light scattering detection (ELSD) and MS/UV. In addition, the compound-buffer solutions used in the various biological assays are quantitated by LC/UV/CLND to determine the concentration of compound actually present during screening. Our results show that LC/UV/CLND/ELSD/MS is a widely applicable method that can be used to purify, quantitate, and identify most small organic molecules from compound libraries. The LC/UV/CLND technique is a simple and sensitive method that can be easily and cost-effectively employed to rapidly determine the concentrations of even small amounts of any N-containing compound in aqueous solution. We present data to establish error limits for concentration determination that are well within the overall variability of the screening process. This study demonstrates that there is a significant difference between the predicted amount of soluble compound from stock DMSO solutions following dilution into assay buffer and the actual amount present in assay buffer solutions, even at the low concentrations employed for the assays. We also demonstrate that knowledge of the concentrations of compounds to which the biological target is exposed is critical for accurate potency determinations. Accurate potency values are in turn particularly important for drug discovery, for understanding structure-activity relationships, and for building useful empirical models of protein-ligand interactions. Our new understanding of relative solubility demonstrates that most, if not all, decisions that are made in early discovery are based upon missing or inaccurate information. Finally, we demonstrate that careful control of compound handling and concentration, coupled with accurate assay methods, allows the use of both positive and negative data in analyzing screening data sets for structure-activity relationships that determine potency and selectivity.
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Breindahl, Torben; Evans-Brown, Michael; Hindersson, Peter; McVeigh, Jim; Bellis, Mark; Stensballe, Allan; Kimergård, Andreas
2015-02-01
New methods were developed and validated to determine the identity, contents, and purity of samples of melanotan II, a synthetic melanocortin receptor agonist, sold in vials as injectable skin-tanning products that were purchased from three online shops. Methods were based on liquid chromatography with ultra-violet detection (LC-UV) at wavelength 218 nm, and tandem mass spectrometric detection (MS/MS) after collision-induced fragmentation of the double charged [M+2H](2+) precursor ion (m/z 513). Identification of melanotan II was verified by correct chromatographic retention time, and relative abundance ratios of five qualifying fragment ions. LC-UV was used to quantify melanotan II as well as impurities. Method validation was performed with reference to guidelines for assessing active substances in authorized medicinal products to reach acceptable accuracy and precision. Vials from two shops contained unknown impurities ranging from 4.1 to 5.9%; impurities from one shop were below the quantification limit. The total amount of melanotan II in vials ranged between 4.32 and 8.84 mg, although each shop claimed that vials contained 10 mg melanotan II. A broad range of drugs used for enhancement purposes can be obtained from the illicit market. However, users of these drugs may be exposed to a range of potential harms, as shown in this study, given that these products are manufactured, distributed and supplied from an illicit market. Copyright © 2014 John Wiley & Sons, Ltd.
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Janssen, Hans-Gerd; Swindells, Chris; Gunning, Philip; Wang, Weijun; Grün, Christian; Mahabir, Krishna; Maharaj, Vinesh J; Apps, Peter J
2008-06-09
High-performance liquid chromatography (HPLC)-UV and HPLC-Mass Spectrometry (MS) methods were developed for the quantitative analysis of the family of Hoodia gordonii steroid glycosides with appetite suppressing properties in dried plant material, in purified and enriched extracts and in various prototype food-products fortified with H. gordonii extracts. For solid materials, e.g. dried plants or for non-fatty foods, extraction of the steroid glycosides is performed using methanol. For products where the steroid glycosides are present in an oil matrix, direct injection of the oil after dilution in tetrahydrofuran is applied. The HPLC separation is performed on an octyl-modified reversed-phase column in the gradient mode with UV detection at lambda = 220 nm. Quantification is performed against an external calibration line prepared using either one of the pure steroid glycosides or geranyl-tiglate. Short- and long-term repeatabilities of the methods are better than 3 and 6%, respectively. Recoveries are better than 85%, even in the analysis of the least abundant steroid glycosides in a complex yoghurt drink. Linearity is better than 3-4 orders of magnitude and the detection limits are below approximately 2 microg g(-1) for the individual steroid glycosides in dried plant material and food products. HPLC-MS is used to confirm that the steroid glycosides contain the characteristic steroid core, the carbohydrate chain and the tigloyl group.
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Varicella-Zoster Virus in Perth, Western Australia: Seasonality and Reactivation
Korostil, Igor A.; Regan, David G.
2016-01-01
Background Identification of the factors affecting reactivation of varicella-zoster virus (VZV) largely remains an open question. Exposure to solar ultra violet (UV) radiation is speculated to facilitate reactivation. Should the role of UV in reactivation be significant, VZV reactivation patterns would generally be expected to be synchronous with seasonal UV profiles in temperate climates. Methods We analysed age and gender specific VZV notification time series data from Perth, Western Australia (WA). This city has more daily sunshine hours than any other major Australian city. Using the cosinor and generalized linear models, we tested these data for seasonality and correlation with UV and temperature. Results We established significant seasonality of varicella notifications and showed that while herpes-zoster (HZ) was not seasonal it had a more stable seasonal component in males over 60 than in any other subpopulation tested. We also detected significant association between HZ notifications and UV for the entire Perth population as well as for females and males separately. In most cases, temperature proved to be a significant factor as well. Conclusions Our findings suggest that UV radiation may be important for VZV reactivation, under the assumption that notification data represent an acceptably accurate qualitative measure of true VZV incidence. PMID:26963841
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NASA Astrophysics Data System (ADS)
Bérces, Attila; ten Kate, I. L.; Fekete, A.; Hegedus, M.; Garry, J. R. C.; Lammer, Helmut; Ehrenfreund, Pascale; Peeters, Zan; Kovacs, G.; Ronto, G.
Mars is considered as a main target for astrobiologically relevant exploration programmes. In order to explain the non-detection of organic material to a detection level of several parts per billion (ppb) by the Viking landers, several hypotheses have been suggested, including degradation processes occurring on the martian surface and in the martian soil and subsurface. UV exposure experiments have been performed in which thin layers of glycine ( 300 nm), and aqueous suspensions of phage T7 and isolated T7 DNA were irradiated with a Deuterium lamp and for comparison with a Xenon arc lamp, modified to simulate the solar irradiation on the surface of Mars (MarsUV). The glycine sample was subjected to 24 hours of irradiation with MarsUV. The results of this glycine experiment show a destruction rate comparable to the results of previous experiments in which thin layers of glycine were irradiated with a deuterium lamp (ten Kate et al., 2005, 2006). After exposure of different doses of simulated Martian UV radiation a decrease of the biological activity of phages and characteristic changes in the UV absorption spectrum have been detected, indicating the UV damage of isolated and intraphage T7 DNA. The results of our experiments show that intraphage DNA is 4 times more sensitive to simulated martian UV and deuterium lamp radiation than isolated T7 DNA. This result indicates the significant role that phage proteins play in the UV damage. The effect of simulated martian radiation is smaller than the biological defects observed after the exposure with a deuterium lamp for both cases, in intraphage and isolated DNA, despite of the 100 times larger intensity of the MarsUV lamp. The detected spectral differences are about ten times smaller; the biological activity is about 3 - 4 times smaller, indicating that the shorter wavelength UV radiation from the deuterium lamp is more effective in inducing DNA damage, irrespective of being intraphage or isolated.
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Au-Pt-Au nanoraspberry structures used for mercury ion detection
NASA Astrophysics Data System (ADS)
Huang, Jiang-Hao; Huang, Shuai; Wen, Xiaoyan; Li, Min; Lu, Haifei
2017-12-01
Detection of Hg2+ with high sensitivity is of great significance in the biochemical sensing field. Quantitative of Hg2+ was realized based on the influence of Hg2+ on the UV-vis absorption performance of Au-Pt-Au core-shell nanoraspberry (APA)-rhodamine-6G (R6G) structure. First, APA sol was added into R6G indicator solution and the UV-vis absorption signal intensity of R6G was evidently promoted. The signal intensity monotonously increased as more APA sol was added. However, when HgCl2 solution was introduced, the signal intensity declined. A linear relationship between Hg2+ concentration and signal intensity at 527 nm was revealed, based on which quantitative determination of Hg2+ could be realized. Hg2+ detection sensitivity was measured to be 0.031 a.u./M with a limit of detection of 10-7 M and the response time was 20 s. A high Hg2+ detection selectivity over Cu2+, Na+, Li+, and K+ was demonstrated. Due to its simplicity and high sensitivity, the proposed method could find an extensive application prospect in the Hg2+ detection field.
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Hellmich, Wibke; Greif, Dominik; Pelargus, Christoph; Anselmetti, Dario; Ros, Alexandra
2006-10-20
Single cell analytics is a key method in the framework of proteom research allowing analyses, which are not subjected to ensemble-averaging, cell-cycle or heterogeneous cell-population effects. Our previous studies on single cell analysis in poly(dimethylsiloxane) microfluidic devices with native label-free laser induced fluorescence detection [W. Hellmich, C. Pelargus, K. Leffhalm, A. Ros, D. Anselmetti, Electrophoresis 26 (2005) 3689] were extended in order to improve separation efficiency and detection sensitivity. Here, we particularly focus on the influence of poly(oxyethylene) based coatings on the separation performance. In addition, the influence on background fluorescence is studied by the variation of the incident laser power as well as the adaptation of the confocal volume to the microfluidic channel dimensions. Last but not least, the use of carbon black particles further enhanced the detection limit to 25 nM, thereby reaching the relevant concentration ranges necessary for the label-free detection of low abundant proteins in single cells. On the basis of these results, we demonstrate the first electropherogram from an individual Spodoptera frugiperda (Sf9) cell with native label-free UV-LIF detection in a microfluidic chip.
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Kendrick, B S; Kerwin, B A; Chang, B S; Philo, J S
2001-12-15
Characterizing the solution structure of protein-polymer conjugates and protein-ligand interactions is important in fields such as biotechnology and biochemistry. Size-exclusion high-performance liquid chromatography with online classical light scattering (LS), refractive index (RI), and UV detection offers a powerful tool in such characterization. Novel methods are presented utilizing LS, RI, and UV signals to rapidly determine the degree of conjugation and the molecular mass of the protein conjugate. Baseline resolution of the chromatographic peaks is not required; peaks need only be sufficiently separated to represent relatively pure fractions. An improved technique for determining the polypeptide-only mass of protein conjugates is also described. These techniques are applied to determining the degree of erythropoietin glycosylation, the degree of polyethylene glycol conjugation to RNase A and brain-derived neurotrophic factor, and the solution association states of these molecules. Calibration methods for the RI, UV, and LS detectors will also be addressed, as well as online methods to determine protein extinction coefficients and dn/dc values both unconjugated and conjugated protein molecules. (c)2001 Elsevier Science.
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Hexagonal-like Nb2O5 Nanoplates-Based Photodetectors and Photocatalyst with High Performances
NASA Astrophysics Data System (ADS)
Liu, Hui; Gao, Nan; Liao, Meiyong; Fang, Xiaosheng
2015-01-01
Ultraviolet (UV) photodetectors are important tools in the fields of optical imaging, environmental monitoring, and air and water sterilization, as well as flame sensing and early rocket plume detection. Herein, hexagonal-like Nb2O5 nanoplates are synthesized using a facile solvothermal method. UV photodetectors based on single Nb2O5 nanoplates are constructed and the optoelectronic properties have been probed. The photodetectors show remarkable sensitivity with a high external quantum efficiency (EQE) of 9617%, and adequate wavelength selectivity with respect to UV-A light. In addition, the photodetectors exhibit robust stability and strong dependence of photocurrent on light intensity. Also, a low-cost drop-casting method is used to fabricate photodetectors based on Nb2O5 nanoplate film, which exhibit singular thermal stability. Moreover, the hexagonal-like Nb2O5 nanoplates show significantly better photocatalytic performances in decomposing Methylene-blue and Rhdamine B dyes than commercial Nb2O5.
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High-throughput technology for novel SO2 oxidation catalysts
Loskyll, Jonas; Stoewe, Klaus; Maier, Wilhelm F
2011-01-01
We review the state of the art and explain the need for better SO2 oxidation catalysts for the production of sulfuric acid. A high-throughput technology has been developed for the study of potential catalysts in the oxidation of SO2 to SO3. High-throughput methods are reviewed and the problems encountered with their adaptation to the corrosive conditions of SO2 oxidation are described. We show that while emissivity-corrected infrared thermography (ecIRT) can be used for primary screening, it is prone to errors because of the large variations in the emissivity of the catalyst surface. UV-visible (UV-Vis) spectrometry was selected instead as a reliable analysis method of monitoring the SO2 conversion. Installing plain sugar absorbents at reactor outlets proved valuable for the detection and quantitative removal of SO3 from the product gas before the UV-Vis analysis. We also overview some elements used for prescreening and those remaining after the screening of the first catalyst generations. PMID:27877427
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Armstrong, Nicholas; Richez, Magali; Raoult, Didier; Chabriere, Eric
2017-08-15
A fast UHPLC-UV method was developed for the simultaneous analysis of Hydroxychloroquine, Minocycline and Doxycycline drugs from 100μL of human serum samples. Serum samples were extracted by liquid-liquid extraction and injected into a phenyl hexyl reverse phase column. Compounds were separated using a mobile phase linear gradient and monitored by UV detection at 343nm. Chloroquine and Oxytetracycline were used as internal standards. Lower and upper limits of quantifications, as well as the other levels of calibration, were validated with acceptable accuracy (<15% deviation) and precision (<15% coefficient of variation) according to the European Medicines Agency guidelines. This new method enables cost and time reduction and was considered suitable for the clinical laboratory. It is the first published assay for the therapeutic drug monitoring of patients diagnosed with Q fever or Whipple's disease. Copyright © 2017 Elsevier B.V. All rights reserved.
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Cyanuric acid (CA) and chloroisocyanurates are commonly used as standard ingredients in formulations for household bleaches, industrial cleansers, dishwasher compounds, general sanitizers, and chlorine stabilizers. They are very well known for preventing the photolytic decomposi...
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Wang, Yan-Hong; Avula, Bharathi; Tang, Wenzhao; Wang, Mei; Elsohly, Mahmoud A; Khan, Ikhlas A
2015-01-01
Stevia products are advertised as a zero-calorie sweetener. Glucose should not be an intrinsic component of this product, but it has been identified from some of stevia products in a preliminary study. An UHPLC-UV method was developed for the quantitative determination of glucose from stevia products. After stevia products reacted with 1-phenyl-3-methyl-5-pyrazolone (PMP), PMP derivatives were analysed and glucose was found in seven out of 35 products in the range 0.3-91.5% (w/w). Two products, SPR-12 and SPR-27, showed remarkable amounts of glucose at 61.6% and 91.5%, respectively. In addition, an UHPLC-UV-evaporative light-scattering detector (ELSD) method was developed for the quantitative determination of rebaudioside A, stevioside, rebaudioside D, dulcoside A and steviolbioside from Stevia rebaudiana and related products. In a 12 min run, five steviol glycosides were baseline-separated. ELSD and ultraviolet (UV) detections showed comparable results. The LC methods were validated for linearity, repeatability, accuracy, limits of detection (LOD) and limits of quantification (LOQ). For steviol glycosides, the LODs and LOQs were found to be less than 10 and 30 μg ml(-1), respectively. The RSD for intra- and inter-day analyses was less than 2.5%, and the recovery was 90-94%. For PMP derivative of glucose, the LOD and LOQ were 0.01 and 0.05 μg ml(-1), respectively. Repeatability (RSD) was less than 2.6%; recovery was 98.6-101.7%. The methods are useful for the identification, quality assurance, and adulterant assessment of S. rebaudiana and steviol glycosides sweeteners (stevia products).
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Kobayashi, Toyohide; Hirose, Jun; Wu, Hong; Sano, Kouichi; Katsumata, Takahiro; Tsujibo, Hiroshi; Nakano, Takashi
2013-12-01
The recent development of antiviral drugs has led to concern that the release of the chemicals in surface water due to expanded medical use could induce drug-resistant mutant viruses in zoonosis. Many researchers have noted that the appearance of an oseltamivir (Tamiflu(®))-resistant avian influenza mutant virus, which may spread to humans, could be induced by oseltamivir contamination of surface water. Although past studies have reported electrolysis as a possible method for degradation of antineoplastics and antibacterials in water, the validity of the method for treatment of antiviral drugs is unknown. In this study, electrolysis was used to degrade an antiviral prodrug, oseltamivir, and a stable active form, oseltamivir carboxylate, and the degradation process was monitored with HPLC-UV and the neuraminidase inhibitory assay. HPLC-UV-detectable oseltamivir and oseltamivir carboxylate were decomposed by electrolysis within 60 min, and inhibitory activity of neuraminidase decreased below the detection limit of the assay used. Cytotoxic and genotoxic activity were not detected in electrolyzed fluid. These results indicate that electrolysis is a possible treatment for inactivation of the antiviral drug oseltamivir. Copyright © 2013 Elsevier B.V. All rights reserved.
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Lee, Yi-Hsuan; Lin, Ying-Chi; Feng, Chia-Hsien; Tseng, Wei-Lung; Lu, Chi-Yu
2017-01-01
4-Hydroxybenzoate is a phenolic derivative of alkyl benzoates and is a widely used preservative in cosmetic and pharmaceutical products. The presence of 4-hydroxybenzoates in the human body may result from the use of pharmaceutical and personal care products. These compounds are also known to exhibit estrogenic and genotoxic activities. The potential adverse effects of these compounds include endocrine disruption, oxidative and DNA damage, contact dermatitis, and allergic reactions. This study used two mass spectrometry methods that are applicable when using a derivatization-enhanced detection strategy (DEDS) to screen 4-hydroxybenzoates and their metabolites. Chemical derivatization was used to enhance the detection of these compounds. To evaluate the metabolic process triggered by UV radiation, human keratinocyte HaCaT cells treated with these 4-hydroxybenzoates were further exposed to UVA, UVB and UVC radiation. Metabolites transformed by human keratinocytes in the chemical derivatization procedure were identified by a nano ultra-performance liquid chromatographic system (nanoUPLC) coupled with LTQ Orbitrap. The experiments confirmed the feasibility of this method for identifying 4-hydroxybenzoate metabolites and for high-throughput screening of 4-hydroxybenzoate in commercial products (50 samples) by the DEDS. PMID:28057923
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Pose-Juan, Eva; Rial-Otero, Raquel; Martínez-Carballo, Elena; López-Periago, Eugenio; Simal-Gándara, Jesús
2009-07-01
Foliar runoff is one of the most important processes affecting off-target movement of fungicides. In this way, Ridomil Gold Plus and Ridomil Gold MZ are two types of wettable powder technical formulations which contain metalaxyl and they are used for such a purpose. A method for quantitative determination of metalaxyl in pesticide formulas has been developed, validated, and subsequently applied to Ridomil Gold Plus and Ridomil Gold MZ. The method employs liquid-liquid extraction followed by liquid chromatography coupled with UV detection (LC-UV), using gas chromatography coupled with mass spectrometry as confirmation technique and to carry out a screening of organic adjuvants of these two selected pesticide formulas. Metalaxyl of 26.5 and 41 g/kg was detected in Ridomil Gold Plus and Ridomil Gold MZ, close to the manufacture specified level of 25 and 40 g/kg, respectively. Activator and utility adjuvants were detected in these two wettable powder technical formulations. Only methyl-ester-based surfactants were found within the group of nonionic surfactants, but the long-term fates of most adjuvants in soils and elsewhere in the environment are largely unknown, partially because of the lack of long-term monitoring data.
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Bahrani, Sonia; Ghaedi, Mehrorang; Dashtian, Kheibar; Ostovan, Abbas; Mansoorkhani, Mohammad Javad Khoshnood; Salehi, Amin
2017-11-01
In present work, facile method is developed for determination of colchicine in human plasma sample, autumn and spring root of colchicium extracts by ultrasound assisted dispersive magnetic solid phase microextraction followed by HPLC-UV method (UAD-MSPME-HPLC-UV). Magnetic (Fe 2 O 4 -nanoparticles) metal organic framework-5, (MOF-5(Zn)-Fe 2 O 4 NPs) was synthesized by dispersing MOF-5 and Fe(NO 3 ) 3 .9H 2 O in ethylene glycol (as capping agent) and NaOH (pH adjustment agent) by hydrothermal method. The prepared sorbent was characterized via XRD and SEM analysis and applied as magnetic solid phase in UAD-MSPME-HPLC-UV method. In this method, colchicine molecules were sorbed on MOF-5(Zn)-Fe 2 O 4 NPs sorbent by various mechanisms like ion exchange, hydrogen bonding and electrostatic, ᴨ-ᴨ, hard-hard and dipole-ion interaction followed by exposing sonication waves as incremental mass transfer agent and then the sorbent was separated from the sample matrix by an external magnetic fields. Subsequently, accumulated colchicine were eluted by small volume of desorption organic solvent. Influence of operational variables such as MOF-5(Zn)-Fe 2 O 4 NPs mass, volume of extracting solvent and sonication time on response property (recovery) were studied and optimized by central composite design (CCD) combined with desirability function (DF) approach. Under optimum condition, the method has wide linear calibration rang (0.5-1700ngmL -1 ) with reasonable detection limit (0.13ngmL -1 ) and R 2 =0.9971. Finally, the UAD-MSPME-HPLC-UV method was successfully applied for determination of colchicine autumn and spring root of colchicium extracts and plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.
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Kahoun, David; Rezková, Sona; Veskrnová, Katerina; Královský, Josef; Holcapek, Michal
2008-08-15
The objective of this study was the determination of 25 phenolic compounds in different mead samples (honeywines) using high performance liquid chromatography (HPLC) with coulometric-array detection and in case of hydroxymethylfurfural with UV detection. Our method was optimized in respect to both the separation selectivity of individual phenolic compounds and the maximum sensitivity with the electrochemical detection. The method development included the optimization of mobile phase composition, the pH value, conditions of the gradient elution and the flow rate using a window-diagram approach. The developed method was used for the determination of limits of detection and limits of quantitation for individual compounds. The linearity of calibration curves, accuracy and precision (intra- and inter-day) at three concentration levels (low, middle and high concentration range) were verified. Mead samples were diluted with the mobile phase at 1:1 to 1:50 ratio depending on the concentration and filtered through a PTFE filter without any other sample pre-treatment. Phenolic compounds concentration was determined in 50 real samples of meads and correlated with meads composition and hydroxymethylfurfural concentration. The most frequently occurred compounds were protocatechuic acid and vanillic acid (both of them were present in 98% samples), the least occurred compounds were (+)-catechin (10% samples) and sinapic acid (12% samples). Vanillin and ethylvanillin, which are used as artificial additives for the taste improvement, were found in 60% and 42% samples, respectively. Hydroxymethylfurfural concentration, as an indicator of honey quality, was in the range from 2.47 to 158 mg/L. Our method is applicable for the determination of 25 phenolic compounds in mead, honey and related natural samples.
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UPLC analysis of free amino acids in wines: profiling of on-lees aged wines.
Fiechter, G; Pavelescu, D; Mayer, H K
2011-05-15
The evolution of free amino acid (FAA) profiles intrinsic to on-lees aged white wines was determined by ultra performance liquid chromatography (UPLC™). On basis of the AccQ.Tag™ method as a commercialized amino acid analysis solution for HPLC, a new protocol for dedicated amino acid analysis using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) for pre-column derivatization was established by method transfer onto UPLC™ conditions. Since AQC derivatives enable both fluorescence (AccQ.Tag™ method) and UV detection, the performed method transfer additionally included changing to a more versatile UV detection. Emphasizing enhanced performance of UPLC™, the newly established protocol facilitated rapid and reliable separations of 24 amino acids within 23 min, hence proved to be superior compared to the original HPLC protocol due to significant improvements in resolution and reduced runtime. Applying UV detection enabled adequate quantifications of AQC amino acid derivatives at μM level (LOQs from 0.12 to 1.10 μM), thus proved sufficient sensitivity for amino acid profiling in wine samples. Moreover, this compiled methodology was successfully applied to monitor the changes of FAA concentrations in four distinct sets of on-lees aged white wines (fermented with different yeasts) at three progressing ripening periods, each (control, 3 and 6 months aging). For the control wines, the applied winery yeast significantly affected total FAA amounts (1450-1740 mg L(-1)). During maturation, the proceeding yeast autolysis implied a rather complex impact on FAAs, yielding total FAA excretions up to 360 mg L(-1). However, the magnitude for increases of specific FAAs (up to +200%) highly depended on the individual amino acids as well as on the applied fermenting yeast. Given the overall complexity of yeast autolysis in winemaking, the application of efficient LC techniques such as UPLC™ may indeed contribute as a valuable tool in wine research for product monitoring and characterization of intrinsic developments during wine maturation. Copyright © 2011 Elsevier B.V. All rights reserved.
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Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar
2017-01-01
Magnetite (Fe 3 O 4 nanoparticles (NPs)) HKUST-1 metal organic framework (MOF) composite as a support was used for surface imprinting of gallic acid imprinted polymer (HKUST-1-MOF-Fe 3 O 4 -GA-MIP) using vinyltrimethoxysilane (VTMOS) as the cross-linker. Subsequently, HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP characterized by FT-IR, XRD and FE-SEM analysis and applied for fast and selective and sensitive ultrasound assisted dispersive magnetic solid phase microextraction of gallic acid (GA) by UV-Vis (UA-DMSPME-UV-Vis) detection method. Plackett-Burman design (PBD) and central composite design (CCD) according to desirability function (DF) indicate the significant variables among the extraction factors vortex (mixing) time (min), sonication time (min), temperature (°C), eluent volume (L), pH and HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP mass (mg) and their contribution on the response. Optimum conditions and values correspond to pH, HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP mass, sonication time and the eluent volume were set as follow 3.0, 1.6mg, 4.0min and 180μL, respectively. The average recovery (ER%) of GA was 98.13% with desirability of 0.997, while the present method has best operational performance like wide linear range 8-6000ngmL -1 with a Limit of detection (LOD) of 1.377ngmL -1 , limit of quantification (LOQ) 4.591ngmL -1 and precision (<3.50% RSD). The recovery of GA in urine, human plasma and water samples within the range of 92.3-100.6% that strongly support high applicability of present method for real samples analysis, which candidate this method as promise for further application. Copyright © 2016. Published by Elsevier B.V.
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John, Harald; Breyer, Felicitas; Schmidt, Christian; Mizaikoff, Boris; Worek, Franz; Thiermann, Horst
2015-10-01
Human butyrylcholinesterase (hBChE) is a serine hydrolase (EC 3.1.1.8) present in all mammalian tissues and the bloodstream. Similar to acetylcholinesterase, the enzyme reacts with organophosphorus compounds (OP) like nerve agents or pesticides that cause enzyme inhibition (BChE adducts). These adducts represent valuable biomarkers for analytical verification of OP exposure. For establishment of these mass spectrometry based methods sufficient amounts of hBChE in high purity are required. Unfortunately, commercial lots are of inappropriate purity thus favouring in-house isolation. Therefore, we developed a small scale procedure to isolate hBChE from citrate plasma. After precipitation by polyethylene glycol (8% w/v and 20% w/v PEG 6000) hBChE was purified from plasma by four consecutive chromatographic steps including anion exchange, affinity extraction and size exclusion. Protein elution was monitored on-line by UV-absorbance (280 nm) followed by continuous fractionation for off-line analysis of (1) hBChE enzyme activity by Ellman assay, (2) protein purity by gel electrophoresis, and (3) protein identity by matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). Numerous major impurities separated from hBChE were identified. The purified material was used for in vitro incubation with diverse OP to establish a μ-liquid chromatography-ultra violet detection/electrospray ionization tandem-mass spectrometric method (μLC-UV/ESI MS/MS) for detection of hBChE adducts suitable for verification analysis. Analytical data for diverse OP pesticides including deuterated analogues as well as G- and V-type nerve agents and their precursor are summarized. This method was successfully applied to plasma samples provided by the Organisation for the Prohibition of Chemical Weapons (OPCW) for the 4th Biomedical Exercise. Copyright © 2015 John Wiley & Sons, Ltd.
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Xiong, Bo; Wang, Ling-Ling; Li, Qiong; Nie, Yu-Ting; Cheng, Shuang-Shuang; Zhang, Hui; Sun, Ren-Qiang; Wang, Yu-Jiao; Zhou, Hong-Bin
2015-11-01
A parallel microscope-based laser-induced fluorescence (LIF), ultraviolet-visible absorbance (UV) and time-of-flight mass spectrometry (TOF-MS) detection for high performance liquid chromatography (HPLC) was achieved and used to determine glucosamine in urines. First, a reliable and convenient LIF detection was developed based on an inverted microscope and corresponding modulations. Parallel HPLC-LIF/UV/TOF-MS detection was developed by the combination of preceding Microscope-based LIF detection and HPLC coupled with UV and TOF-MS. The proposed setup, due to its parallel scheme, was free of the influence from photo bleaching in LIF detection. Rhodamine B, glutamic acid and glucosamine have been determined to evaluate its performance. Moreover, the proposed strategy was used to determine the glucosamine in urines, and subsequent results suggested that glucosamine, which was widely used in the prevention of the bone arthritis, was metabolized to urines within 4h. Furthermore, its concentration in urines decreased to 5.4mM at 12h. Efficient glucosamine detection was achieved based on a sensitive quantification (LIF), a universal detection (UV) and structural characterizations (TOF-MS). This application indicated that the proposed strategy was sensitive, universal and versatile, and it was capable of improved analysis, especially for analytes with low concentrations in complex samples, compared with conventional HPLC-UV/TOF-MS. Copyright © 2015 Elsevier B.V. All rights reserved.
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Pyka, Alina; Budzisz, Marika; Dołowy, Małgorzata
2013-01-01
Adsorption thin layer chromatography (NP-TLC) with densitometry has been established for the identification and the quantification of acetaminophen in three leading commercial products of pharmaceutical tablets coded as brand: P1 (Product no. 1), P2 (Product no. 2), and P3 (Product no. 3). Applied chromatographic conditions have separated acetaminophen from its related substances, namely, 4-aminophenol and and 4′-chloroacetanilide. UV densitometry was performed in absorbance mode at 248 nm. The presented method was validated by specificity, range, linearity, accuracy, precision, detection limit, quantitative limit, and robustness. The TLC-densitometric method was also compared with a pharmacopeial UV-spectrophotometric method for the assay of acetaminophen, and the results confirmed statistically that the NP-TLC-densitometric method can be used as a substitute method. It could be said that the validated NP-TLC-densitometric method is suitable for the routine analysis of acetaminophen in quantity control laboratories. PMID:24063006
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NASA Astrophysics Data System (ADS)
Abdulrahman, Sameer A. M.; Basavaiah, K.; Cijo, M. X.; Vinay, K. B.
2012-11-01
Spectrophotometric methods have been developed for the determination of dothiepin hydrochloride (DOTH) in both pure and tablet dosage form and their limits of detection and quantification have been evaluated. The methods are based on the measurement of the absorbance of a DOTH solution either in 0.1 N HCl at 229 nm (method A) or in methanol at 231 nm (method B). Beer's law is obeyed over a concentration range of 1-16 μg/ml DOTH for both methods. Molar absorptivity values are calculated to be 2.48 × 104 and 2.42 × 104 l/(mol × cm) with Sandell sensitivity values of 0.0134 and 0.0137 μg/cm2 for methods A and B, respectively. The degradation behavior of DOTH was investigated under different stress conditions such as acid hydrolysis, alkaline hydrolysis, water hydrolysis, oxidation, dry heat treatment, and UV-degradation. The drug undergoes significant degradation under oxidative conditions only.
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Nestola, Marco; Thellmann, Andrea
2015-01-01
An online normal-phase liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS) method was developed for the determination of vitamins D2 and D3 in selected food matrices. Transfer of the sample from HPLC to GC was realized by large volume on-column injection; detection was performed with a time-of-flight mass spectrometer (TOF-MS). Typical GC problems in the determination of vitamin D such as sample degradation or sensitivity issues, previously reported in the literature, were not observed. Determination of total vitamin D content was done by quantitation of its pyro isomer based on an isotopically labelled internal standard (ISTD). Extracted ion traces of analyte and ISTD showed cross-contribution, but non-linearity of the calibration curve was not determined inside the chosen calibration range by selection of appropriate quantifier ions. Absolute limits of detection (LOD) and quantitation (LOQ) for vitamins D2 and D3 were calculated as approximately 50 and 150 pg, respectively. Repeatability with internal standard correction was below 2 %. Good agreement between quantitative results of an established high-performance liquid chromatography with UV detection (HPLC-UV) method and HPLC-GC-MS was found. Sterol-enriched margarine was subjected to HPLC-GC-MS and HPLC-MS/MS for comparison, because HPLC-UV showed strong matrix interferences. HPLC-GC-MS produced comparable results with less manual sample cleanup. In summary, online hyphenation of HPLC and GC allowed a minimization in manual sample preparation with an increase of sample throughput.
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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.
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Prior, Amir; Coliva, Giulia; de Jong, Gerhardus J; Somsen, Govert W
2018-05-29
The potential of capillary electrophoresis (CE) with ultraviolet (UV)-excited fluorescence detection for sensitive chiral analysis of amino acids (AAs) was investigated. DL-AAs were derivatized with 9-fluorenylmethoxycarbonyl chloride (FMOC)-Cl to allow their fluorescence detection and enhance enantioseparation. Fluorescence detection was achieved employing optical fibers, leading UV excitation light (< 300 nm) from a Xe-Hg lamp to the capillary window, and fluorescence emission to a spectrograph equipped with a charge-coupled device (CCD). Signal averaging over time and emission wavelength intervals was carried out to improve the signal-to-noise ratio of the FMOC-AAs. A background electrolyte (BGE) of 40 mM sodium tetraborate (pH 9.5), containing 15% isopropanol (v/v), 30 mM sodium dodecyl sulfate (SDS), and 30 mM β-cyclodextrin (β-CD), was found optimal for AA chemo- and enantioseparation. Enantioresolutions of 1.0 or higher were achieved for 16 proteinogenic DL-AAs. Limits of detection (LODs) were in the 10-100-nM range (injected concentration) for the D-AA enantiomers, except for FMOC-D-tryptophan (536 nM) which showed intramolecular fluorescence quenching. Linearity (R 2 > 0.997) and repeatability for peak height (relative standard deviations (RSDs) < 7.0%; n = 5) and electrophoretic mobility (RSDs < 0.6%; n = 5) of individual AA enantiomers were established for chiral analysis of DL-AA mixtures. The applicability of the method was investigated by the analysis of cerebrospinal fluid (CSF). Next to L-AAs, endogenous levels of D-glutamine and D-aspartic acid could be measured in CSF revealing enantiomeric ratios of 0.35 and 19.6%, respectively. This indicates the method's potential for the analysis of low concentrations of D-AAs in presence of abundant L-AAs.
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Ruan, Yudi; Wu, Lie; Jiang, Xiue
2016-05-23
Water-soluble nitrogen-doped carbon nanoparticles (N-CNPs) prepared by the one-step hydrothermal treatment of uric acid were found to show ratiometric changes in their UV-vis spectra due to Hg(2+)-mediated self-assembly. For the first time, such a property was developed into a UV-vis optical sensor for detecting Hg(2+) in aqueous solutions with high sensitively and selectively (detection limit = 1.4 nM). More importantly, this novel sensor exhibits a higher linear sensitivity over a wider concentration range compared with the fluorescence sensor based on the same N-CNPs. This work opens an exciting new avenue to explore the use of carbon nanoparticles in constructing UV-vis optical sensors for the detection of metal ions and the use of carbon nanoparticles as a new building block to self-assemble into superlattices.
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[Effect of ultraviolet radiation on ALDH1 expression in human lens epithelial cells].
Shi, Jingming; Jia, Songbai; Chen, Xuan; Tang, Luosheng
2012-06-01
To determine the apoptosis-inducing effect of ultraviolet light (UV) on human lens epithelial cell (HLEC) and to explore the involvement of changes in ALDH1 folowing UV radiation. HLEC was exposed to the same UV light source and was subsequently divided into 6 groups according to UV radiation time of 0 (control group), 5, 10, 15, and 30 min. Apoptosis was detected by AO/EB staining. Changes of ALDH1 in HLEC were detected by immunohistochemical staining and Western blot. The intensity of immunohistochemical staining and the rate of positive cells decreased with increase of UV time (P<0.05). The rate of positive ALDH1 cells was negatively correlated with the rate of apoptosis (r= -0.92, P<0.05). Western blot showed the integrated absorbance values significantly decreased with the increase of UV time (P<0.05). ALDH1 in HLEC decreases with an increase of UV exposure, which may be related to UV induced apoptosis of HLEC.
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The chitosan - Porphyrazine hybrid materials and their photochemical properties.
Chełminiak-Dudkiewicz, Dorota; Ziegler-Borowska, Marta; Stolarska, Magdalena; Sobotta, Lukasz; Falkowski, Michal; Mielcarek, Jadwiga; Goslinski, Tomasz; Kowalonek, Jolanta; Węgrzynowska-Drzymalska, Katarzyna; Kaczmarek, Halina
2018-04-01
Three magnesium sulfanyl porphyrazines differing in the size of peripheral substituents (3,5-dimethoxybenzylsulfanyl, (3,5-dimethoxybenzyloxy)benzylsulfanyl, 3,5-bis[(3,5-bis[(3,5-dimethoxybenzyloxy)benzyloxy]benzylsulfanyl) were exposed to visible and ultraviolet radiation (UV A + B + C) in order to determine their photochemical properties. The course of photochemical reactions in dimethylformamide solutions and the ability of the systems to generate singlet oxygen were studied by UV-Vis spectroscopy, which additionally gave information on aggregation processes. The porphyrazines were found to be stable upon visible light irradiation conditions, but when exposed to high energy UV radiation, the efficient photodegradation of these macrocycles was observed. Therefore, these three magnesium sulfanyl porphyrazines were incorporated into chitosan matrix. The obtained thin films of chitosan doped with porphyrazines were subjected to polychromatic UV-radiation and studied by spectroscopic methods (UV-Vis, FTIR), scanning electron microscopy (SEM) and atomic force microscopy (AFM). Application of chitosan as a polymer matrix for porphyrazines was found to be successful method that effectively stopped the unwelcome degradation of macrocycles, thus worth considering for their photoprotection. In addition, the surface properties of the hybrid material were determined by contact angle measurements and calculation of surface free energy. Intermolecular interactions between these novel porphyrazines and chitosan were detected. The mechanism of photochemical reactions occurring in studied systems has been discussed. Copyright © 2018 Elsevier B.V. All rights reserved.
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Wingfield, Jenna L.; Ruane, Lauren G.; Patterson, Joshua D.
2017-01-01
Premise of the study: The three-dimensional structure of tree canopies creates environmental heterogeneity, which can differentially influence the chemistry, morphology, physiology, and/or phenology of leaves. Previous studies that subdivide canopy leaves into broad categories (i.e., “upper/lower”) fail to capture the differences in microenvironments experienced by leaves throughout the three-dimensional space of a canopy. Methods: We use a three-dimensional spatial mapping approach based on spherical polar coordinates to examine the fine-scale spatial distributions of photosynthetically active radiation (PAR) and the concentration of ultraviolet (UV)-absorbing compounds (A300) among leaves within the canopies of black mangroves (Avicennia germinans). Results: Linear regressions revealed that interior leaves received less PAR and produced fewer UV-absorbing compounds than leaves on the exterior of the canopy. By allocating more UV-absorbing compounds to the leaves on the exterior of the canopy, black mangroves may be maximizing UV-protection while minimizing biosynthesis of UV-absorbing compounds. Discussion: Three-dimensional spatial mapping provides an inexpensive and portable method to detect fine-scale differences in environmental and biological traits within canopies. We used it to understand the relationship between PAR and A300, but the same approach can also be used to identify traits associated with the spatial distribution of herbivores, pollinators, and pathogens. PMID:29188145
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Cloud point extraction of Δ9-tetrahydrocannabinol from cannabis resin.
Ameur, S; Haddou, B; Derriche, Z; Canselier, J P; Gourdon, C
2013-04-01
A cloud point extraction coupled with high performance liquid chromatography (HPLC/UV) method was developed for the determination of Δ(9)-tetrahydrocannabinol (THC) in micellar phase. The nonionic surfactant "Dowfax 20B102" was used to extract and pre-concentrate THC from cannabis resin, prior to its determination with a HPLC-UV system (diode array detector) with isocratic elution. The parameters and variables affecting the extraction were investigated. Under optimum conditions (1 wt.% Dowfax 20B102, 1 wt.% Na2SO4, T = 318 K, t = 30 min), this method yielded a quite satisfactory recovery rate (~81 %). The limit of detection was 0.04 μg mL(-1), and the relative standard deviation was less than 2 %. Compared with conventional solid-liquid extraction, this new method avoids the use of volatile organic solvents, therefore is environmentally safer.
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USDA-ARS?s Scientific Manuscript database
Vitamin D3 (cholecalciferol) levels were determined in finfish and shellfish using UV detection at 265nm (combined with auxiliary full scan UV detection) and selected ion monitoring (SIM) mass spectrometry (MS), using vitamin D2 (ergocalciferol) as an internal standard. Analysis of standard referen...
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[Simultaneous determination of 6 neonicotinoid residues in soil using DLLME-HPLC and UV].
Sun, Bao-li; Shan, Hong; Li, Yan-hua; Zeng, Ya-ling; Shen, Xiu-li; Tong, Cheng-feng
2013-09-01
A simple, cheap and rugged method was developed for simultaneous deter mination of 6 neonicotinoid residues in soil, including imidacloprid, acetamiprid, thiamethoxam, thiacloprid, clothianidin and nitenpyram. The soil sample was produced by dispersive liquid-liquid micro-extraction (DLLME) after extracted by the mixed solution of acetonitrile and CH2Cl2 (2:1, phi). The analytes were separated by HPLC with Alltima C18 column (4.6 mm x 250 mm, 5 microm) and detected by PDA at 260 nm. External standard method was used for quantification. The results showed that good linearity was obtained with correlation coefficients between 0.9982 and 0.9999 in the range of 0.5-200 microg x L(-1). The limits of detection (LODs) were in the range between 0.0005 and 0.003 microg x mL(-1) (S/N = 3). The method was validated with five soil samples spiked at three fortification levels (0.05, 0.1, 1.0 mg x kg(-1)) and recoveries were in the range of 55.3%-95.6% with RSD of 1.4%-7.0%. The effect of clean-up was evaluated by UV spectra and demonstrated that the method established is effective. In conclusion, this method is competent for the simultaneous analysis of 6 neonicotinoid residues in soil.
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Determination of Trace Level Triclosan in Water by Online Preconcentration and HPLC-UV Diode Array
An online high performance liquid chromatography (HPLC) method for the detection and quantification of trace levels of triclosan in water is discussed. Triclosan, an anti-bacterial agent, and related compounds have been shown to reach municipal waste waters through the disposal ...
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2012-02-24
AND SUBTITLE Detection of Biochemical Pathogens, Laser Stand-off Spectroscopy, Quantum Coherence, and Many Body Quantum Optics 6. AUTHORS Marian O...Maximum 200 words) Results of our earlier research in the realm of quantum optics were extended in order to solve the challenging technical problems of...efficient methods of generating UV light via quantum coherence. 14. SUBJECT TERMS Quantum coherence, quantum optics, lasers 15. NUMBER OF PAGES 15
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Couderc, François; Ong-Meang, Varravaddheay; Poinsot, Véréna
2017-01-01
Native laser-induced fluorescence using UV lasers associated to CE offers now a large related literature, for now 30 years. The main works have been performed using very expensive Ar-ion lasers emitting at 257 and 275 nm. They are not affordable for routine analyses, but have numerous applications such as protein, catecholamine, and indolamine analysis. Some other lasers such as HeCd 325 nm have been used but only for few applications. Diode lasers, emitting at 266 nm, cheaper, are extensively used for the same topics, even if the obtained sensitivity is lower than the one observed using the costly UV-Ar-ion lasers. This review presents various CE or microchips applications and different UV lasers used for the excitation of native fluorescence. We showed that CE/Native UV laser induced fluorescence detection is very sensitive for detection as well as small aromatic biomolecules than proteins containing Trp and Tyr amino acids. Moreover, it is a simple way to analyze biomolecules without derivatization. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Development of an ion mobility spectrometer with UV ionization source to detect ketones and BTX
NASA Astrophysics Data System (ADS)
Ni, Kai; Guo, Jingran; Ou, Guangli; Lei, Yu; Wang, Xiaohao
2014-11-01
Ion mobility spectrometry (IMS) is an attractive material analysis technology for developing a miniaturized volatile organic compounds (VOCs) on-site monitoring sensor. Having simple instrumentation, IMS is especially suitable when portability and sensitivity are required. In this work, we designed an ion mobility spectrometer with UV ionization. The geometric parameters of the UV-IMS were optimized based on a numerical simulation. The simulation results demonstrated that the drift electric field in the drift region was approximately homogenous and in the reaction region had an ion focusing effect, which could improve the sensitivity and resolving power of the IMS. The UV-IMS has been constructed and used to detect VOCs, such as acetone, benzene, toluene and m-xylene (BTX). The resolution of these substance measured from the UV-IMS in the atmospheric conditions are about 30 and the limit of detection (LOD) is low to ppmv. The ion mobility module and electric circuit are integrated in a main PCB, which can facilitate mass production and miniaturization. The present UV-IMS is expected to become a tool of choice for the on-site monitoring for VOCs.
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2.0 SUMMARY OF METHOD
2.1 In both TOC and DOC determinations, organic carbon in the water sample is oxidized to form carbon dioxide (CO2), which is then measured by a detection system. There are two different approaches for the oxidation of organic carbon in water sample... -
Tang, Shisong; Vinerot, Nataly; Fisher, Danny; Bulatov, Valery; Yavetz-Chen, Yehuda; Schechter, Israel
2016-08-01
Multiphoton electron extraction spectroscopy (MEES) is an analytical method in which UV laser pulses are utilized for extracting electrons from solid surfaces in multiphoton processes under ambient conditions. Counting the emitted electrons as a function of laser wavelength results in detailed spectral features, which can be used for material identification. The method has been applied to detection of trace explosives on a variety of surfaces. Detection was possible on dusty swabs spiked with explosives and also in the standard dry-transfer contamination procedure. Plastic explosives could also be detected. The analytical limits of detection (LODs) are in the sub pmole range, which indicates that MEES is one of the most sensitive detection methods for solid surface under ambient conditions. Scanning the surface with the laser allows for its imaging, such that explosives (as well as other materials) can be located. The imaging mode is also useful in forensic applications, such as detection of explosives in human fingerprints. Copyright © 2016 Elsevier B.V. All rights reserved.
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Toal, Sarah J; Sanchez, Jason C; Dugan, Regina E; Trogler, William C
2007-01-01
The detection of trace explosives is important for forensic, military, and homeland security applications. Detection of widely used nitroaromatic explosives (trinitrotoluene [TNT], 2,4-dinitrotoluene [DNT], picric acid [PA]) was carried out using photoluminescent metallole-containing polymers. The method of detection is through the quenching of fluorescence of thin films of the polymer, prepared by spray coating organic solutions of the polymer, by the explosive analyte. Visual quenching of luminescence (lambda(em) approximately 400-510 nm) in the presence of the explosive is seen immediately upon illumination with near-UV light (lambda(ex)=360 nm). Detection limits were observed to be as low as 5 ng for TNT, 20 ng for DNT, and 5 ng for PA. In addition, experiments with normal production line explosives and their components show that this technology is also able to detect composition B, Pyrodex, and nitromethane. This method offers a convenient and sensitive method of detection of trace nitroaromatic explosive residue.
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He, Ke; Timm, Anne; Blaney, Lee
2017-08-04
Ultraviolet-filters (UV-filters) and estrogens have attracted increased attention as contaminants of emerging concern (CECs) due to their widespread occurrence in the environment. Most of these CECs are hydrophobic and have the potential to accumulate in aquatic organisms. To date, co-analysis of UV-filters and estrogens has not been reported due, in part, to the complex environmental matrices. Here, a multi-residue method has been developed for simultaneous determination of five UV-filters and three estrogens in tissue from aquatic and marine organisms. The procedure involved a modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction with a novel reverse-solid-phase extraction (reverse-SPE) cleanup in place of dispersive-SPE, followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis. The tissue mass, acetonitrile content, and salt conditions for QuEChERS extraction, along with the reverse-SPE cartridge material and elution conditions, were thoroughly investigated and optimized. Five UV-filters (i.e., 3-(4-methylbenzylidene) camphor, benzophenone-3, ethylhexylmethoxycinnamate, homosalate, and octocrylene) and three estrogens (i.e., estrone, 17β-estradiol, and 17α-ethinylestradiol) were simultaneously analyzed by taking advantage of wrong-way-round ionization in LC-MS/MS. The optimized analytical protocol exhibited good recoveries (>80%) for target compounds and enabled their detection at concentrations as low as 0.2ng/g in 50mg tissue samples. The method was applied to determine concentrations of target analytes in four invertebrates (i.e., Orconectes virilis, Procambarus clarkii, Crassostrea virginica, and Ischadium recurvum). All eight target analytes were detected at least once in the tissue samples, with the highest concentration being 399ng/g of homosalate in O. virilis. These results highlight the ubiquitous bioaccumulation of CECs in aquatic and marine invertebrates. Copyright © 2017 Elsevier B.V. All rights reserved.
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The secrets of T Pyxidis. I. UV observations
NASA Astrophysics Data System (ADS)
Gilmozzi, R.; Selvelli, P.
2007-01-01
Aims:We study the UV spectral behavior of the recurrent nova T Pyx during 16 years of
IUE observations. Methods: We examined both theIUE line-by-line images and the extracted spectra in order to understand the reality and the origin of the observed spectral variations. We compare different extraction methods and their influence on the spectrum of an extended object. Results: The UV continuum of T Pyx has remained nearly constant in slope and intensity over this time interval, without any indication of long-term trends. The reddening determined from the UV data is EB-V=0.25 ± 0.02. The best single-curve fit to the dereddened UV continuum is a power-law distribution ∝λ-2.33. The tail of this curve agrees well with the B, V, and J magnitudes of T Pyx, indicating that the contribution of the secondary star is negligible. One peculiar aspect of T Pyx is that most emission lines (the strongest ones being those of CIV 1550 and HeII 1640) show substantial changes both in intensity and detectability, in contrast to the near constancy of the continuum. Several individual spectra display emission features that are difficult to identify, suggesting a composite spectroscopic system. We tentatively ascribe the origin of these transient emission features either to loops and jets from the irradiated secondary or to moving knots of the surrounding nebula that are (temporarily) projected in front of the system. The inspection of all IUE line-by-line images has led to the detection of emission spikes outside the central strip of the spectrum, which in some cases seem associated to known emission features in the (main) spectrum. A comparison with other ex-novae reveals a surprising similarity to the spectrum of the very-slow nova HR Del, whose white dwarf primary has a mass that is allegedly about one half that of T Pyx. -
Xu, Hui; Jia, Li
2009-01-01
A capillary liquid chromatography (CLC) system with UV/vis detection was coupled with an in-tube solid-phase microextraction (SPME) device for the analysis of fat-soluble vitamins and beta-carotene. A monolithic silica-ODS column was used as the extraction medium. An optical-fiber flow cell with a long light path in the UV/vis detector was utilized to further enhance the detection sensitivity. In the in-tube SPME/CLC system, the pre-condition of the extraction column and the effect of the injection volume were investigated. The detection limits (LOD) for the fat-soluble vitamins and beta-carotene were in the range from 1.9 to 173 ng/mL based on the signal-to-noise ratio of 3 (S/N=3). The relative standard deviations of migration time and peak area for each analyte were less than 5.0%. The method was applied to the analysis of fat-soluble vitamins and beta-carotene contents in corns.
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Akl, Magda A; Ahmed, Mona A; Ramadan, Ahmed
2011-05-15
In pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipments and areas. The cleaning procedures must be validated and methods to determine trace amounts of drugs have, therefore, to be considered with special attention. An HPLC-UV method for the determination of ceftriaxone sodium residues on stainless steel surface was developed and validated in order to control a cleaning procedure. Cotton swabs, moistened with extraction solution (50% water and 50% mobile phase), were used to remove any residues of drugs from stainless steel surfaces, and give recoveries of 91.12, 93.8 and 98.7% for three concentration levels. The precision of the results, reported as the relative standard deviation (RSD), were below 1.5%. The method was validated over a concentration range of 1.15-6.92 μg ml(-1). Low quantities of drug residues were determined by HPLC-UV using a Hypersil ODS 5 μm (250×4.6 mm) at 50 °C with an acetonitrile:water:pH 7:pH 5 (39-55-5.5-0.5) mobile phase at flow rate of 1.5 ml min(-1), an injection volume of 20 μl and were detected at 254 nm. A simple, selective and sensitive HPLC-UV assay for the determination of ceftriaxone sodium residues on stainless steel surfaces was developed, validated and applied. Copyright © 2011 Elsevier B.V. All rights reserved.
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Mohamed, S; Flint, S; Palmer, J; Fletcher, G C; Pitt, J I
2013-09-01
A simple and rapid screening method was developed for the detection of citrinin in fungal cultures using Coconut Cream Agar (CCA) described previously for detecting aflatoxin and ochratoxin A. Fifteen isolates of Penicillium citrinum were inoculated onto CCA and incubated at 25 and 30°C for 10 days. All isolates produced a distinct yellow green fluorescence on CCA when the reverse side of the agar plates were viewed under long wavelength UV light. Detection was optimal at 25°C after four to 5 days of incubation. Isolates positive by the CCA method also tested positive for citrinin production by the TLC agar plug method after growth on CCA, Czapek yeast extract agar and yeast extract sucrose agar. Control cultures were negative by both methods, indicating that the CCA Petri dish method was suitable for screening cultures for citrinin production. © 2013 The Society for Applied Microbiology.
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Murillo Pulgarín, José A; García Bermejo, Luisa F; Sánchez García, M Nieves
2011-01-01
A sensitive chemiluminescence method for vitamin B(12) using a charge-coupled device (CCD) photodetector combined with on-line UV-persulfate oxidation in a simple continuous flow system has been developed. The principle for the determination of vitamin B(12) is based on the enhancive effect of cobalt (II) on the chemiluminescence reaction between luminol and percarbonate in alkaline medium. In addition, percarbonate has been investigated and proposed as a powerful source of hydrogen peroxide as oxidant agent in this chemiluminescence reaction. The digestion of vitamin B(12) to release the cobalt (II) is reached by UV irradiation treatment in a persulfate medium. The CCD detector, directly connected to the flow cell, is used with the continuous flow manifold to obtain the full spectral characteristics of cobalt (II) catalyzed luminol-percarbonate reaction. The vitamin B(12) oxidation process and chemical conditions for the chemiluminescence reaction were investigated and optimized. The increment of the emission intensity was proportional to the concentration of vitamin B(12) , giving a second-order calibration graph over the cobalt (II) concentration range from 10 to 5000 μg L(-1)(r(2) = 0.9985) with a detection limit of 9.3 μg L(-1). The proposed method was applied to the determination of vitamin B(12) in different kinds of pharmaceuticals. Copyright © 2011 John Wiley & Sons, Ltd.
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Zhang, Pingping; Lian, Kaoqi; Wu, Xiaoli; Yao, Min; Lu, Xin; Kang, Weijun; Jiang, Lingling
2014-04-04
Determining the level of urinary 8-hydroxy-2'-deoxyguanosine (8-OHdG), an oxidative DNA damage biomarker, is vital to the study of clinical pathogenesis and drug toxicity. The principal limitation of capillary electrophoresis (CE) with UV detection is its low sensitivity. To overcome this shortcoming, we developed a micellar electrokinetic capillary chromatography (MEKC) with solid-phase extraction (SPE) for urinary 8-OHdG analysis. The sensitivity of MEKC-UV was improved using a reasonable UV system, injection mode, and SPE. The parameters affecting MEKC and SPE were also optimized. The calibration curve was linear within the range from 1 to 500 μg L(-1). The limits of detection and quantification were 0.27 μg L(-1) and 0.82 μg L(-1), respectively. Interday and intraday precision were both <5.6%. The recovery of 8-OHdG in urine ranged from 94.5% to 103.2%. This method was used to measure urinary 8-OHdG from eight normal children, eight newly diagnosed leukemic children, and eight leukemic children undergoing chemotherapy. The results show that the proposed method can be used to assess oxidative stress in patients and the side effects of chemotherapeutic drugs by measuring urinary 8-OHdG. Copyright © 2014 Elsevier B.V. All rights reserved.
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Lech, Katarzyna; Jarosz, Maciej
2011-03-01
High-performance liquid chromatography coupled with spectrophotometric and electrospray mass spectrometric detection (HPLC-UV-Vis-ESI MS) was used for characterization of natural dyes present in historical art works. The gradient program was developed for identification of 29 colorants of various polarities. Dual detection system (UV-Vis and ESI MS) allowed differentiation of all compounds, even if they were not completely separated. This enabled examination of more color compounds over a substantially shorter time in comparison with previously recommended methods. Moreover, for extraction of colorants from historical textiles a two-step sequential procedure was proposed, excluding evaporation used in earlier procedures. The developed method was successfully applied to identification of indigotin, carminic, kermesic, flavokermesic, dcII, dcIV, dcVII, and ellagic acids as well as luteolin, apigenin, and genistein in red, violet, and green fibers taken from three selected historical chasubles which belong to the collection of the Wawel Cathedral treasury (Cracow, Poland). Italian textiles from the fifteenth and sixteenth centuries, of which chasubles were made, were dyed with a limited number of dyestuffs, consistently used for all batches of fabrics. The obtained results also allowed confirmation of the structure of the so-called "dcII" component of cochineal as a C-glucose derivative of flavokermesic acid.
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Ulloa, A; Rodríguez, M H; Rodríguez, A D; Roberts, D R
1997-09-01
The abundance and age structure of Anopheles albimanus populations were estimated by UV updraft light traps and human landing catches within villages and in nearby breeding sites of southern México. Four villages and 5 breeding sites were selected for the study. Light trap and human landing catches were simultaneously carried out in each breeding site and each village. Anopheles albimanus was the most abundant malaria vector caught in breeding sites and in villages. Significant differences in overall An. albimanus abundance among villages and among breeding sites were detected only by human landing catches. In both villages and breeding sites, more mosquitoes were captured by 1 human bait (34.3 +/- 6.3 and 14.6 +/- 2.9, respectively) than by one light trap (15.9 +/- 3.3 and 2.4 +/- 0.3 respectively) collection. After pooling, no significant differences were detected in the abundance estimated by each method in breeding sites and villages. A significant correlation of numbers of specimens between methods was detected. Age structure was different between samples from breeding sites and villages, with more gravid females collected in breeding sites, whereas more nulipars were collected in villages. By collection method, age structure was also different both in breeding sites and in villages. In breeding sites, the percentage of parous females was significantly higher in human landing catches, whereas the percentage of gravid females was significantly higher in light traps. In villages, only the percentage of gravid females was significantly higher in light traps. Our results suggests that UV light traps could be used to measure several entomological parameters of An. albimanus populations because both abundance variations and parity rates were similarly detected by both methods.
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NASA Astrophysics Data System (ADS)
Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel
2012-03-01
A novel, selective, sensitive and simple spectrophotometric method was developed and validated for the determination of the antidepressant duloxetine hydrochloride in pharmaceutical preparation. The method was based on the reaction of duloxetine hydrochloride with 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline media to yield orange colored product. The formation of this complex was also confirmed by UV-visible, FTIR, 1H NMR, Mass spectra techniques and thermal analysis. This method was validated for various parameters according to ICH guidelines. Beer's law is obeyed in a range of 5.0-60 μg/mL at the maximum absorption wavelength of 480 nm. The detection limit is 0.99 μg/mL and the recovery rate is in a range of 98.10-99.57%. The proposed methods was validated and applied to the determination of duloxetine hydrochloride in pharmaceutical preparation. The results were statistically analyzed and compared to those of a reference UV spectrophotometric method.
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Zidan, Dalia W; Hassan, Wafaa S; Elmasry, Manal S; Shalaby, Abdalla A
2018-06-01
Simultaneous determination of sofosbuvir (SOF), and daclatasvir (DAC) in their dosage forms, human urine and human plasma using simple and rapid micellar high performance liquid chromatographic method coupled with UV detection (HPLC-UV) had been developed and validated. These drugs are described as co-administered for treatment of Hepatitis C virus (HCV). HCV is the cause of Hepatitis C and some cancers such as liver cancer (hepatocellular carcinoma) and lymphomas in humans. Separation and quantitation were carried out on anonyx™ C 8 monolithic (100 × 4.6 mm (i.d.) analytical column maintained at 25 °C. The mobile phase consisted of 0.1 M sodium dodecyl sulfate (SDS) solution containing 20% (V/V) n-propanolol and 0.3% (V/V) triethylamine and pH was adjusted to 6.5 using 0.02 M phosphoric acid, respectively. The retention times of SOF and DAC were 4.8 min, and 6.5 min, respectively. Measurements were made at flow rate of 0.5 mL/min with injection volume of 20 μL and ultraviolet (UV) detection at 226 nm. Linearity of SOF and DAC was obtained over concentration ranges of 50-400, and 40-400 ng/mL, respectively in pure form, 60-300 and 50-300 ng/mL, respectively for human plasma and over 50-400, and 40-400 ng/mL, respectively for human urine with correlation coefficient >0.999. The proposed method demonstrated excellent intra- and inter-day precision and accuracy. The suggested method was applied for determination of the drugs in pure, dosage form, and in real human plasma, real human urine and drug-dissolution test of their tablets. The obtained results have been statistically compared to reported method to give a conclusion that there is no significant differences. Copyright © 2018 Elsevier B.V. All rights reserved.
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Raghavan, Rahul; Cheriyamundath, Sanith; Madassery, Joseph
2015-01-01
Objectives: To investigate the effect of DMSO on cisplatin induced cytotoxicity (invitro) against K562 (Human mylogenous leukemia) cell line and to study the cisplatin-DMSO adduct formation using UV-spectrophotometer. Materials and methods: Effect of DMSO on the cytotoxicity of cisplatin was studied in K562 (Chronic mylogenous leukemia) cell line by MTT assay. Cisplatin-DMSO adduct formation was studied by continuously monitoring the increase in absorption peaks for 30 minutes using UV-spectrophotometer. Results: 0.1-0.3% DMSO markedly reduced the cytotoxic activity of cisplatin in K562 cells. Cisplatin-DMSO adduct formation was detected using UV-spectrophotometer. Continuous increase in UV absorbance between 250nm-290nm was observed when cisplatin (0.5mg/ml) and DMSO (10%) were mixed. Conclusion: Present study revealed that DMSO inactivates the cytotoxicity of cisplatin. Cisplatin-DMSO mixture showed increased absorbance at 250-290nm. Therefore, using DMSO in invitro assays might result in misinterpretation of actual efficacy of drugs. PMID:26069372
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Kandelbauer, A; Kessler, W; Kessler, R W
2008-03-01
The laccase-catalysed transformation of indigo carmine (IC) with and without a redox active mediator was studied using online UV-visible spectroscopy. Deconvolution of the mixture spectra obtained during the reaction was performed on a model-free basis using multivariate curve resolution (MCR). Thereby, the time courses of educts, products, and reaction intermediates involved in the transformation were reconstructed without prior mechanistic assumptions. Furthermore, the spectral signature of a reactive intermediate which could not have been detected by a classical hard-modelling approach was extracted from the chemometric analysis. The findings suggest that the combined use of UV-visible spectroscopy and MCR may lead to unexpectedly deep mechanistic evidence otherwise buried in the experimental data. Thus, although rather an unspecific method, UV-visible spectroscopy can prove useful in the monitoring of chemical reactions when combined with MCR. This offers a wide range of chemists a cheap and readily available, highly sensitive tool for chemical reaction online monitoring.
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Carranco, Núria; Farrés-Cebrián, Mireia; Saurina, Javier
2018-01-01
High performance liquid chromatography method with ultra-violet detection (HPLC-UV) fingerprinting was applied for the analysis and characterization of olive oils, and was performed using a Zorbax Eclipse XDB-C8 reversed-phase column under gradient elution, employing 0.1% formic acid aqueous solution and methanol as mobile phase. More than 130 edible oils, including monovarietal extra-virgin olive oils (EVOOs) and other vegetable oils, were analyzed. Principal component analysis results showed a noticeable discrimination between olive oils and other vegetable oils using raw HPLC-UV chromatographic profiles as data descriptors. However, selected HPLC-UV chromatographic time-window segments were necessary to achieve discrimination among monovarietal EVOOs. Partial least square (PLS) regression was employed to tackle olive oil authentication of Arbequina EVOO adulterated with Picual EVOO, a refined olive oil, and sunflower oil. Highly satisfactory results were obtained after PLS analysis, with overall errors in the quantitation of adulteration in the Arbequina EVOO (minimum 2.5% adulterant) below 2.9%. PMID:29561820
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Pedras, M Soledade C; Adio, Adewale M; Suchy, Mojmir; Okinyo, Denis P O; Zheng, Qing-An; Jha, Mukund; Sarwar, Mohammed G
2006-11-10
We have analyzed 23 crucifer phytoalexins (e.g. brassinin, dioxibrassinin, cyclobrassinin, brassicanals A and C) by HPLC with diode array detection and electrospray ionization mass spectrometry (HPLC-DAD-ESI-MS) using both negative and positive ion modes. Positive ion mode ESI-MS appeared more sensitive than negative ion mode ESI-MS in detecting this group of compounds. A new HPLC separation method, new LC-MS and LC-MS(2) data and proposed fragmentation pathways, LC retention times, and UV spectra for selected compounds are reported.
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Franco, Pedro H C; Chellini, Paula R; Oliveira, Marcone A L; Pianetti, Gerson A
2017-07-01
Tuberculosis is the second most deadly infectious disease, surpassed only by HIV/AIDS, and has resulted in over 1 billion deaths in the last 200 years. The World Health Organization estimates that in 2014, 9.6 million people were infected by this disease and 1.5 million had died. First-choice treatment consists of fixed-dose combination tablets containing rifampicin, isoniazid, pyrazinamide, and ethambutol hydrochloride (4-FDC). There are pharmacopeial protocols available to test 4-FDC, but they are prolonged, two-step methods. One single-step method in the literature performs the simultaneous determination by HPLC, but requires a long acquisition time. In this context, an ultra-HPLC (UHPLC) method was developed based on the HPLC method with the objective of reducing analysis time. A C18 column (1.9 µm particle size) was used with UV-diode-array detection at 238 and 282 nm. The method was found to be selective, linear, exact, precise, and robust. Samples from two batches were analyzed and the results compared with those obtained by the HPLC method, with no statistically significant differences observed (P > 0.05). This UHPLC method reduced the analysis time from 17 to 4 min, with a more than 90% reduction in sample and reagent consumption and a financial economy of almost 50-fold.
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Sugawara, Jun; Kou, Seiko; Kou, Sousei; Yasumura, Kazunori; Satake, Toshihiko; Maegawa, Jiro
2015-02-01
Laser "toning" with a Q-switched neodymium-doped yttrium aluminum garnet (Nd:YAG) laser has recently been described to be effective for the treatment of melasma. Leukoderma is a refractory complication of laser toning for melasma, but it can be detected early with ultraviolet (UV) imaging. We assessed the relationship between leukoderma and the frequency or total number of laser toning sessions, as well as the effectiveness of UV imaging for detecting leukoderma. The subjects included 147 patients who received at least five laser toning sessions. Subjects were classified into three groups according to the frequency of treatment (weekly for Group A1, fortnightly for Group A2, and monthly for Group B), and the incidence of leukoderma was compared among the three groups. In patients who developed leukoderma, the interval between clinical diagnosis and leukoderma detection on UV images (obtained with a Visia Evolution during every laser toning session) was determined to evaluate the effectiveness of UV imaging for the early detection of leukoderma. The overall incidence of leukoderma was 2% (3/147 patients): 3.8% (1/26 patients) in Group A1, 4% (2/49 patients) in Group A2, and 0% (0/72 patients) in Group B. There were no significant differences in the incidence of leukoderma relative to the frequency of laser toning. In two of the three patients who developed leukoderma, it was diagnosed clinically at the 20th and 21st laser toning session, whereas it was diagnosed by UV imaging at the 12th and 13th session. In the remaining 1 patient, leukoderma was detected clinically and by UV imaging at the 7th session. There was no significant difference in the incidence of leukoderma related to the frequency of laser toning. This study showed that there are two types of leukoderma associated with laser toning. UV imaging was effective for the early detection of type 1 leukoderma, which seems to be related to the cumulative laser energy delivered, but not for detecting type 2 leukoderma, which may be due to direct phototoxicity. © 2015 Wiley Periodicals, Inc.
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NASA Astrophysics Data System (ADS)
Maity, Anupam; Panda, Sovan Kumar
2018-04-01
Reddish-yellow color colloid consisting of silver nanoparticles (Ag NPs) has been synthesized by reducing aqueous AgNO3 solution by photo-induced citrate reduction technique under UV light. As prepared colloid exhibits single and intense plasmonic absorption peak in the violet region of the visible spectra with the peak centered at 405 nm. The NPs are fine and spherical with diameter ranging from 5 to 10 nm. These colloidal NPs have been used for the quantitative detection of uric acid by UV-VIS spectroscopy. A linear red shifting of the characteristics Plasmonic absorption peak of Ag NPs is observed with uric acid concentration. Uric acid can be detected by UV-VIS spectroscopy down to 5 nM limit using the prepared colloid.
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An infectious enteric adenovirus was isolated from urban wastewater receiving tertiary treatment and ultraviolet (UV) disinfection. A pilot study was undertaken to investigate the efficacy of UV disinfection (low pressure, high intensity radiation) of total and fecal coliform bac...
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Aspartate Aminotransferase (AST/GOT) and Alanine Aminotransferase (ALT/GPT) Detection Techniques
Huang, Xing-Jiu; Choi, Yang-Kyu; Im, Hyung-Soon; Yarimaga, Oktay; Yoon, Euisik; Kim, Hak-Sung
2006-01-01
The levels of aspartate aminotransferase (AST/GOT) and alanine aminotransferase (ALT/GPT) in serum can help people diagnose body tissues especially the heart and the liver are injured or not. This article provides a comprehensive review of research activities that concentrate on AST/GOT and ALT/GPT detection techniques due to their clinical importance. The detection techniques include colorimetric, spectrophotometric, chemiluminescence, chromatography, fluorescence and UV absorbance, radiochemical, and electrochemical techniques. We devote the most attention on experimental principle. In some methods a few representative devices and important conclusions are presented.
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NASA Astrophysics Data System (ADS)
Qi, Yingying; Li, Li; Li, Baoxin
2009-09-01
A simple and sensitive label-free colorimetric detection of telomere DNA has been developed. It was based on the color change of gold nanoparticles (AuNPs) due to DNA hybridization. UV-vis spectra and transmission electron microscopy (TEM) were used to investigate the change of AuNPs. Under the optimized conditions, the linear range for determination of telomere DNA was 5.7 × 10 -13 to 4.5 × 10 -6 mol/L. The detection limit (3 σ) of this method has decreased to pico-molar level.
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Wang, Zhijiang; Wu, Lina; Shen, Baozhong; Jiang, Zhaohua
2013-09-30
Fluorescent detection is an attractive method for the detection of toxic chemicals. However, most chemosensors that are currently utilized in fluorescent detection are based on organic dyes or quantum dots, which suffer from instability, high background noise and interference from organic impurities in solution, which can also be excited by UV radiation. In the present research, we developed a novel NaYF4:Yb,Ho/Au nanocomposite-based chemosensor with high sensitivity (10 ppb) and selectivity over competing analytes for the detection of the insecticide cartap. This nanosensor is excited with a 970-nm laser instead of UV radiation to give an emission peak at 541 nm. In the presence of cartap, the nanocomposites aggregate, resulting in enhanced luminescence resonance energy transfer between the NaYF4:Yb,Ho nanocrystals and the gold nanoparticles, which decreases the emission intensity at 541 nm. The relative luminescence intensity at 541 nm has a linear relationship with the concentration of cartap in the solution. Based on this behavior, the developed nanosensor successfully detected cartap in farm produce and water samples with satisfactory results. Copyright © 2013 Elsevier B.V. All rights reserved.
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Jeong, Birang; Roh, Jong Seong; Yoon, Michung; Yoon, Yoosik; Shin, Soon Shik; Cho, Hyun Joo; Kwon, Yong Soo; Yang, Heejung
2018-01-01
Background: DF formula is a herbal preparation comprised three medicinal herbs, namely, Ephedra intermedia, Rheum palmatum, and Lithospermum erythrorhizon, which is being used for the treatment of obesity and liver fibrosis in Korean local clinics. Objective: Since the abovementioned three herbs exist with different proportions in DF formula and their chemical markers have different physiochemical properties; it is quite challenging to develop an analytical methodology for the determination of these chemical markers. Materials and Methods: For the analysis of the three herbs, five chemicals, (+)-pseudoephedrine (1) and (−)-ephedrine (2) for E. intermedia, aloe-emodin (3), and chrysophanol (4) for R. palmatum, and shikonin (5) for L. erythrorhizon, were selected for method validation of DF formula, and the analytical conditions were optimized and validated using high-performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). Results: The specificities for the five compounds 1–5 were determined by their UV absorption spectra (1–4: 215 nm and 5: 520 nm). Their calibration curves showed good linear regressions with high correlation coefficient values (R2 > 0.9997). The limits of detection of these five markers were in the range 0.4–2.1 ng/mL, with the exception of 5 (12.7 ng/mL). The intraday variability for all the chemical markers was less than a Relative standard deviation (RSD) of 3%, except for 5 (RSD = 12.6%). In the case of interday analysis, 1 (1.0%), 2 (3.1%), and 4 (3.7%) showed much lower variabilities (RSD < 5%) than 3 (7.6%) and 5 (8.2%). Moreover, the five chemical markers showed good recoveries with good accuracies in the range of 90%–110%. Conclusions: The developed HPLC-UV method for the determination of the five chemical markers of the components of DF formula was validated. SUMMARY DF formula, the herbal composition of Ephedra intermedia, Rheum palmatum and Lithospermum erythrorhizonFive chemical markers in DF formula were (+)-pseudoephedrine (1) and (-)-ephedrine (2) for E. intermedia, aloe-emodin (3) and chrysopanol (4) for R. palmatum, and shikonin (5) for L. erythrorhizon, with quite different physico-chemical propertiesFive chemical markers in DF formula were determined by HPLC-UV Abbreviations used: EP: (−)-ephedrine; PSEP: (+)-pseudoephedrine; HPLC: High-performance liquid chromatography; UV: Ultraviolet; LOD: Limit of detection; LOQ: Limit of quantification; RSD: Relative standard deviation. PMID:29720825
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McMahon, Gillian; Wall, Rachel; Nolan, Kieran; Diamond, Dermot
2002-07-19
A series of derivatisation reactions between p-t-butyl calix[4]arene and ethyl bromoacetate were carried out in order to prepare 1,3 diester substituted calix[4]arene. Mass spectral data, obtained from direct injection of samples, indicated that the reactions were rich in the desired product. Since the ultra violet (UV) spectra of the desired product and possible impurities are very similar, liquid chromatography (LC) chromatographic data seemed to corroborate these results. However, when on-line LC-UV-MS was carried out and each LC peak subjected to MS analysis as it eluted, a very different picture emerged. It was found that many of these reactions actually contained high levels of the monoester product which, having less affinity for sodium in the MS, is therefore seriously underestimated in any direct injection assay. LC-diode array detection (DAD) methods were also used to help successfully identify and characterise the compounds being formed in these complex reactions. The overall results obtained in this paper allowed the optimal reaction conditions to be determined for this reaction. LC-MS analysis of the chromatographic peaks also identified the presence of two isomers of the diester substituted calix[4]arene (1,3 and 1,2 diesters). The combination of LC and UV/MS detection is required for accurate analysis of the products of such reactions.
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NASA Astrophysics Data System (ADS)
Rohit, Jigneshkumar V.; Kailasa, Suresh Kumar
2014-11-01
We have developed a simple and rapid colorimetric method for on-site analysis of thiram and paraquat using cyclen dithiocarbamate-functionalized silver nanoparticles (CN-DTC-Ag NPs) as a colorimetric probe. The synthesized CN-DTC-Ag NPs were characterized by UV-Visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy, dynamic light scattering, and transmission electron microscopic techniques. The CN-DTC molecules provide good supramolecular self assembly on the surfaces of Ag NPs to encapsulate thiram and paraquat selectively via "host-guest" chemistry, resulting in red-shift in surface plasmon resonance peak of CN-DTC-Ag NPs from 396 to 530 nm and 510 nm and color change from yellow to pink for thiram and to orange for paraquat, which can be naked-eye detected. The present method shows good linearity in the range of 10.0-20.0 µM and of 50.0-250 µM with limits of detection 2.81 × 10-6 M and 7.21 × 10-6 M for thiram and paraquat, respectively. This method was proved as a promising tool for on-site and real-time monitoring of thiram and paraquat in environmental water, potato, and wheat samples.
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Metal-Insulator-Semiconductor Photodetectors
Lin, Chu-Hsuan; Liu, Chee Wee
2010-01-01
The major radiation of the Sun can be roughly divided into three regions: ultraviolet, visible, and infrared light. Detection in these three regions is important to human beings. The metal-insulator-semiconductor photodetector, with a simpler process than the pn-junction photodetector and a lower dark current than the MSM photodetector, has been developed for light detection in these three regions. Ideal UV photodetectors with high UV-to-visible rejection ratio could be demonstrated with III–V metal-insulator-semiconductor UV photodetectors. The visible-light detection and near-infrared optical communications have been implemented with Si and Ge metal-insulator-semiconductor photodetectors. For mid- and long-wavelength infrared detection, metal-insulator-semiconductor SiGe/Si quantum dot infrared photodetectors have been developed, and the detection spectrum covers atmospheric transmission windows. PMID:22163382
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NASA Astrophysics Data System (ADS)
Wang, Yanfang; Yang, Na; Liu, Yi
2018-04-01
A novel organic small molecule with D-Pi-A structure was prepared, which was found to be a promising colorimetric and ratiometric UV-vis spetral probe for detection of phosphorylated proteins with the help of tetravalent zirconium ion. Such optical probe based on chromophore WYF-1 shows a rapid response (within 10 s) and high selectivity and sensitivity for phosphorylated proteins, giving distinct colorimetric and ratiometric UV-vis changes at 720 and 560 nm. The detection limit for phosphorylated proteins was estimated to be 100 nM. In addition, detection of phosphorylated proteins in placental tissue samples with this probe was successfully applied, which indicates that this probe holds great potential for phosphorylated proteins detection.
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Douglas, Leisa; MacKinnon, Gillian; Cook, Gordon; Duncan, Harry; Briddon, Adrian; Seamark, Steven
2018-03-01
Isopropyl-N-(3-chlorophenyl) carbamate (CIPC, common name Chlorpropham) is commonly used for post-harvest sprout inhibition in stored potatoes. It is applied as a thermal fog which results in loss to the fabric of the store and the atmosphere. Recently, there have been concerns in the United Kingdom because of cross contamination of other crop commodities that were stored in buildings with a history of CIPC usage. This cross contamination may have occurred because of retained residues in the fabric of the stores. The retention of CIPC in concrete is poorly understood; therefore the requirement for a robust analytical method for the detection and quantification of CIPC in concrete is a critical first step in tackling this problem. A method using High-Performance Liquid Chromatography with ultraviolet detection (HPLC UV/VIS) was validated. CIPC recoveries at three concentration levels (0.4, 4.0 and 40.0 μg g -1 ) were in the range of 90.7-97.0% with relative standard deviations between 2.14 and 3.01%. The limits of detection and quantification were 0.03 and 0.1 μg g -1 , respectively. This study confirmed that CIPC was persistent in concrete to a depth of 4 cm, with >90% within the top 1 cm of the flooring. Copyright © 2017 Elsevier Ltd. All rights reserved.
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Quantification of active principles and pigments in leaf extracts of Isatis tinctoria by HPLC/UV/MS.
Mohn, Tobias; Potterat, Olivier; Hamburger, Matthias
2007-02-01
An HPLC method has been developed and validated for the quantification of the pharmacologically active principles tryptanthrin (1), 1,3-dihydro-3-[(4-hydroxy-3,5-dimethoxyphenyl)methylene]-2 H-indol-2-one (indolinone) (3), indirubin (4), alpha-linolenic acid (2), and indigo (5), an isomer of indirubin, in extracts from the traditional anti-inflammatory plant Isatis tinctoria (woad). The chromatographic separation was performed on a C-18 column with a linear gradient of acetonitrile in water containing 0.1% formic acid. The method combines UV and electrospray MS detection in the positive ion mode for the detection of the alkaloids, with a switch to the negative mode for the analysis of alpha-linolenic acid. The method was applied to the analysis of woad extracts obtained by supercritical fluid (SFE) CO2 extraction, and by pressurized liquid extraction (PLE) with dichloromethane and methanol, respectively. While the highest concentration of alpha-linolenic acid was found in the SFE extract (7.43%), the concentrations of tryptanthrin , indolinone, indirubin and indigo were the highest in the dichloromethane extract (0.30, 0.035, 2.48 and 0.84%, respectively). Compound 3 was not detected in the methanolic extract and only traces of compounds 1, 4 and 5 and low amount of alpha-linolenic acid (0.39%) were present in this extract.
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Hybrid AlGaN-SiC Avalanche Photodiode for Deep-UV Photon Detection
NASA Technical Reports Server (NTRS)
Aslam, Shahid; Herrero, Federico A.; Sigwarth, John; Goldsman, Neil; Akturk, Akin
2010-01-01
The proposed device is capable of counting ultraviolet (UV) photons, is compatible for inclusion into space instruments, and has applications as deep- UV detectors for calibration systems, curing systems, and crack detection. The device is based on a Separate Absorption and Charge Multiplication (SACM) structure. It is based on aluminum gallium nitride (AlGaN) absorber on a silicon carbide APD (avalanche photodiode). The AlGaN layer absorbs incident UV photons and injects photogenerated carriers into an underlying SiC APD that is operated in Geiger mode and provides current multiplication via avalanche breakdown. The solid-state detector is capable of sensing 100-to-365-nanometer wavelength radiation at a flux level as low as 6 photons/pixel/s. Advantages include, visible-light blindness, operation in harsh environments (e.g., high temperatures), deep-UV detection response, high gain, and Geiger mode operation at low voltage. Furthermore, the device can also be designed in array formats, e.g., linear arrays or 2D arrays (micropixels inside a superpixel).
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Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A
2000-02-11
The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.
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Fanali, Chiara; Dugo, Laura; D'Orazio, Giovanni; Lirangi, Melania; Dachà, Marina; Dugo, Paola; Mondello, Luigi
2011-01-01
Nano-LC and conventional HPLC techniques were applied for the analysis of anthocyanins present in commercial fruit juices using a capillary column of 100 μm id and a 2.1 mm id narrow-bore C(18) column. Analytes were detected by UV-Vis at 518 nm and ESI-ion trap MS with HPLC and nano-LC, respectively. Commercial blueberry juice (14 anthocyanins detected) was used to optimize chromatographic separation of analytes and other analysis parameters. Qualitative identification of anthocyanins was performed by comparing the recorded mass spectral data with those of published papers. The use of the same mobile phase composition in both techniques revealed that the miniaturized method exhibited shorter analysis time and higher sensitivity than narrow-bore chromatography. Good intra-day and day-to-day precision of retention time was obtained in both methods with values of RSD less than 3.4 and 0.8% for nano-LC and HPLC, respectively. Quantitative analysis was performed by external standard curve calibration of cyanidin-3-O-glucoside standard. Calibration curves were linear in the concentration ranges studied, 0.1-50 and 6-50 μg/mL for HPLC-UV/Vis and nano-LC-MS, respectively. LOD and LOQ values were good for both methods. In addition to commercial blueberry juice, qualitative and quantitative analysis of other juices (e.g. raspberry, sweet cherry and pomegranate) was performed. The optimized nano-LC-MS method allowed an easy and selective identification and quantification of anthocyanins in commercial fruit juices; it offered good results, shorter analysis time and reduced mobile phase volume with respect to narrow-bore HPLC. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Papandreou, Georgios; Zorpas, Kostas; Archontaki, Helen
2011-11-01
Simultaneous determination of aniracetam and its related impurities (2-pyrrolidinone, p-anisic acid, 4-p-anisamidobutyric acid and (p-anisoyl)-4-methyl-2-pyrrolidinone) was accomplished in the bulk drug and in a tablet formulation using a high performance liquid chromatographic method with UV detection. Separation was achieved on a Hypersil BDS-CN column (150 mm × 4.0 mm, 5 μm) using a gradient elution program with solvent A composed of phosphate buffer (pH 4.0; 0.010 M) and solvent B of acetonitrile-phosphate buffer (pH 4.0; 0.010 M) (90:10, v/v). The flow rate of the mobile phase was 1.0 mL min(-1) and the total elution time, including the column re-equilibration, was approximately 20 min. The UV detection wavelength was varied appropriately among 210, 250 and 280 nm. Injection volume was 20 μL and experiments were conducted at ambient temperature. The developed method was validated in terms of system suitability, selectivity, linearity, range, precision, accuracy, limits of detection and quantification for the impurities, short term and long term stability of the analytes in the prepared solutions and robustness, following the ICH guidelines. Therefore, the proposed method was suitable for the simultaneous determination of aniracetam and its studied related impurities. Copyright © 2011 Elsevier B.V. All rights reserved.
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Bord, N; Crétier, G; Rocca, J-L; Bailly, C; Souchez, J-P
2004-09-01
Alkanolamines such as diethanolamine (DEA) and N-methyldiethanolamine (MDEA) are used in desulfurization processes in crude oil refineries. These compounds may be found in process waters following an accidental contamination. The analysis of alkanolamines in refinery process waters is very difficult due to the high ammonium concentration of the samples. This paper describes a method for the determination of DEA in high ammonium concentration refinery process waters by using capillary electrophoresis (CE) with indirect UV detection. The same method can be used for the determination of MDEA. Best results were achieved with a background electrolyte (BGE) comprising 10 mM histidine adjusted to pH 5.0 with acetic acid. The development of this electrolyte and the analytical performances are discussed. The quantification was performed by using internal standardization, by which triethanolamine (TEA) was used as internal standard. A matrix effect due to the high ammonium content has been highlighted and standard addition was therefore used. The developed method was characterized in terms of repeatability of migration times and corrected peak areas, linearity, and accuracy. Limits of detection (LODs) and quantification (LOQs) obtained were 0.2 and 0.7 ppm, respectively. The CE method was applied to the determination of DEA or MDEA in refinery process waters spiked with known amounts of analytes and it gave excellent results, since uncertainties obtained were 8 and 5%, respectively.
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Taheri, Salman; Jalali, Fahimeh; Fattahi, Nazir; Jalili, Ronak; Bahrami, Gholamreza
2015-10-01
Dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the extraction of methadone and determination by high-performance liquid chromatography with UV detection. In this method, no microsyringe or fiber is required to support the organic microdrop due to the usage of an organic solvent with a low density and appropriate melting point. Furthermore, the extractant droplet can be collected easily by solidifying it at low temperature. 1-Undecanol and methanol were chosen as extraction and disperser solvents, respectively. Parameters that influence extraction efficiency, i.e. volumes of extracting and dispersing solvents, pH, and salt effect, were optimized by using response surface methodology. Under optimal conditions, enrichment factor for methadone was 134 and 160 in serum and urine samples, respectively. The limit of detection was 3.34 ng/mmL in serum and 1.67 ng/mL in urine samples. Compared with the traditional dispersive liquid-liquid microextraction, the proposed method obtained lower limit of detection. Moreover, the solidification of floating organic solvent facilitated the phase transfer. And most importantly, it avoided using high-density and toxic solvents of traditional dispersive liquid-liquid microextraction method. The proposed method was successfully applied to the determination of methadone in serum and urine samples of an addicted individual under methadone therapy. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Degradation of microbial fluorescence biosignatures by solar ultraviolet radiation on Mars
NASA Astrophysics Data System (ADS)
Dartnell, Lewis R.; Patel, Manish R.
2014-04-01
Recent and proposed robotic missions to Mars are equipped with implements to expose or excavate fresh material from beneath the immediate surface. Once brought into the open, any organic molecules or potential biosignatures of present or past life will be exposed to the unfiltered solar ultraviolet (UV) radiation and face photolytic degradation over short time courses. The key question, then, is what is the window of opportunity for detection of recently exposed samples during robotic operations? Detection of autofluorescence has been proposed as a simple method for surveying or triaging samples for organic molecules. Using a Mars simulation chamber we conduct UV exposures on thin frozen layers of two model microorganisms, the radiation-resistant polyextremophile Deinococcus radiodurans and the cyanobacterium Synechocystis sp. PCC 6803. Excitation-emission matrices (EEMs) are generated of the full fluorescence response to quantify the change in signal of different cellular fluorophores over Martian equivalent time. Fluorescence of Deinococcus cells, protected by a high concentration of carotenoid pigments, was found to be relatively stable over 32 h of Martian UV irradiation, with around 90% of the initial signal remaining. By comparison, fluorescence from protein-bound tryptophan in Synechocystis is much more sensitive to UV photodegradation, declining to 50% after 64 h exposure. The signal most readily degraded by UV irradiation is fluorescence of the photosynthetic pigments - diminished to only 35% after 64 h. This sensitivity may be expected as the biological function of chlorophyll and phycocyanin is to optimize the harvesting of light energy and so they are readily photobleached. A significant increase in a ~450 nm emission feature is interpreted as accumulation of fluorescent cellular degradation products from photolysis. Accounting for diurnal variation in Martian sunlight, this study calculates that frozen cellular biosignatures would remain detectable by fluorescence for at least several sols; offering a sufficient window for robotic exploration operations.
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Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie
2016-12-21
The sample matrix can enhance the gas chromatography signal of pesticide residues relative to that obtained with the same concentration of pesticide in solvent. This paper is related to negative matrix effects observed in coupled gas chromatography-mass spectrometry ion trap (GC/MS 2 ) quantification of pesticides in concentrated extracts of apple peel prepared by the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method. It is focused on the pesticides most frequently used on the apple varieties studied, throughout the crop cycle, right up to harvest, to combat pests and diseases and to improve fruit storage properties. Extracts from the fleshy receptacle (flesh), the epiderm (peel) and fruit of three apple varieties were studied by high-performance thin-layer chromatography hyphenated with UV-vis light detection (HPTLC/UV visible). The peel extracts had high concentrations of triterpenic acids (oleanolic and ursolic acids), reaching 25mgkg -1 , whereas these compounds were not detected in the flesh extracts (<0.05mgkg -1 ). A significant relationship has been found between the levels of these molecules and negative matrix effects in GC/MS 2 . The differences in the behavior of pesticides with respect to matrix effects can be accounted for by the physicochemical characteristics of the molecules (lone pairs, labile hydrogen, conjugation). The HPTLC/UV visible method developed here for the characterization of QuEChERS extracts acts as a complementary clean-up method, aimed to decrease the negative matrix effects of such extracts. Copyright © 2016 Elsevier B.V. All rights reserved.
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Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie
2017-02-03
The sample matrix can enhance the gas chromatography signal of pesticide residues relative to that obtained with the same concentration of pesticide in solvent. This paper is related to negative matrix effects observed in coupled gas chromatography-mass spectrometry ion trap (GC/MS 2 ) quantification of pesticides in concentrated extracts of apple peel prepared by the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method. It is focused on the pesticides most frequently used on the apple varieties studied, throughout the crop cycle, right up to harvest, to combat pests and diseases and to improve fruit storage properties. Extracts from the fleshy receptacle (flesh), the epiderm (peel) and fruit of three apple varieties were studied by high-performance thin-layer chromatography hyphenated with UV-vis light detection (HPTLC/UV visible). The peel extracts had high concentrations of triterpenic acids (oleanolic and ursolic acids), reaching 25mgkg -1 , whereas these compounds were not detected in the flesh extracts (<0.05mgkg -1 ). A significant relationship has been found between the levels of these molecules and negative matrix effects in GC/MS 2 . The differences in the behavior of pesticides with respect to matrix effects can be accounted for by the physicochemical characteristics of the molecules (lone pairs, labile hydrogen, conjugation). The HPTLC/UV visible method developed here for the characterization of QuEChERS extracts acts as a complementary clean-up method, aimed to decrease the negative matrix effects of such extracts. Copyright © 2016 Elsevier B.V. All rights reserved.
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NASA Astrophysics Data System (ADS)
Mabood, Fazal; Hussain, Z.; Haq, H.; Arian, M. B.; Boqué, R.; Khan, K. M.; Hussain, K.; Jabeen, F.; Hussain, J.; Ahmed, M.; Alharasi, A.; Naureen, Z.; Hussain, H.; Khan, A.; Perveen, S.
2016-01-01
A new UV-Visible spectroscopic method assisted with microwave for the determination of glucose in pharmaceutical formulations was developed. In this study glucose solutions were oxidized by ammonium molybdate in the presence of microwave energy and reacted with aniline to produce a colored solution. Optimum conditions of the reaction including wavelength, temperature, and pH of the medium and relative concentration ratio of the reactants were investigated. It was found that the optimal wavelength for the reaction is 610 nm, the optimal reaction time is 80 s, the optimal reaction temperature is 160 °C, the optimal reaction pH is 4, and the optimal concentration ratio aniline/ammonium molybdate solution was found to be 1:1. The limits of detection and quantification of the method are 0.82 and 2.75 ppm for glucose solution, respectively. The use of microwaves improved the speed of the method while the use of aniline improved the sensitivity of the method by shifting the wavelength.
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Single Photon Counting UV Solar-Blind Detectors Using Silicon and III-Nitride Materials
Nikzad, Shouleh; Hoenk, Michael; Jewell, April D.; Hennessy, John J.; Carver, Alexander G.; Jones, Todd J.; Goodsall, Timothy M.; Hamden, Erika T.; Suvarna, Puneet; Bulmer, J.; Shahedipour-Sandvik, F.; Charbon, Edoardo; Padmanabhan, Preethi; Hancock, Bruce; Bell, L. Douglas
2016-01-01
Ultraviolet (UV) studies in astronomy, cosmology, planetary studies, biological and medical applications often require precision detection of faint objects and in many cases require photon-counting detection. We present an overview of two approaches for achieving photon counting in the UV. The first approach involves UV enhancement of photon-counting silicon detectors, including electron multiplying charge-coupled devices and avalanche photodiodes. The approach used here employs molecular beam epitaxy for delta doping and superlattice doping for surface passivation and high UV quantum efficiency. Additional UV enhancements include antireflection (AR) and solar-blind UV bandpass coatings prepared by atomic layer deposition. Quantum efficiency (QE) measurements show QE > 50% in the 100–300 nm range for detectors with simple AR coatings, and QE ≅ 80% at ~206 nm has been shown when more complex AR coatings are used. The second approach is based on avalanche photodiodes in III-nitride materials with high QE and intrinsic solar blindness. PMID:27338399
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Single Photon Counting UV Solar-Blind Detectors Using Silicon and III-Nitride Materials.
Nikzad, Shouleh; Hoenk, Michael; Jewell, April D; Hennessy, John J; Carver, Alexander G; Jones, Todd J; Goodsall, Timothy M; Hamden, Erika T; Suvarna, Puneet; Bulmer, J; Shahedipour-Sandvik, F; Charbon, Edoardo; Padmanabhan, Preethi; Hancock, Bruce; Bell, L Douglas
2016-06-21
Ultraviolet (UV) studies in astronomy, cosmology, planetary studies, biological and medical applications often require precision detection of faint objects and in many cases require photon-counting detection. We present an overview of two approaches for achieving photon counting in the UV. The first approach involves UV enhancement of photon-counting silicon detectors, including electron multiplying charge-coupled devices and avalanche photodiodes. The approach used here employs molecular beam epitaxy for delta doping and superlattice doping for surface passivation and high UV quantum efficiency. Additional UV enhancements include antireflection (AR) and solar-blind UV bandpass coatings prepared by atomic layer deposition. Quantum efficiency (QE) measurements show QE > 50% in the 100-300 nm range for detectors with simple AR coatings, and QE ≅ 80% at ~206 nm has been shown when more complex AR coatings are used. The second approach is based on avalanche photodiodes in III-nitride materials with high QE and intrinsic solar blindness.
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Gürkan, Ramazan; Kır, Ufuk; Altunay, Nail
2015-08-01
The determination of inorganic arsenic species in water, beverages and foods become crucial in recent years, because arsenic species are considered carcinogenic and found at high concentrations in the samples. This communication describes a new cloud-point extraction (CPE) method for the determination of low quantity of arsenic species in the samples, purchased from the local market by UV-Visible Spectrophotometer (UV-Vis). The method is based on selective ternary complex of As(V) with acridine orange (AOH(+)) being a versatile fluorescence cationic dye in presence of tartaric acid and polyethylene glycol tert-octylphenyl ether (Triton X-114) at pH 5.0. Under the optimized conditions, a preconcentration factor of 65 and detection limit (3S blank/m) of 1.14 μg L(-1) was obtained from the calibration curve constructed in the range of 4-450 μg L(-1) with a correlation coefficient of 0.9932 for As(V). The method is validated by the analysis of certified reference materials (CRMs). Copyright © 2015 Elsevier Ltd. All rights reserved.
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Determination of boldine in plasma by high-performance liquid chromatography.
Speisky, H; Cassels, B K; Nieto, S; Valenzuela, A; Nuñez-Vergara, L J
1993-02-26
A sensitive method for the determination of boldine in blood plasma is described. The procedure involves a direct pH-buffered chloroform extraction of boldine from blood plasma, followed by its assay under isocratic conditions by HPLC with UV detection. The extraction recovery is excellent, and sensitivity and precision of the method are very high, when applied to plasma samples containing pharmacologically relevant concentrations of boldine.
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Kääriä, K; Hirvonen, A; Norppa, H; Piirilä, P; Vainio, H; Rosenberg, C
2001-04-01
Occupational exposure to 4,4'-methylenediphenyl diisocyanate (MDI) was measured during moulding of rigid polyurethane foam. The aim of the study was to find out whether an MDI-derived urinary amine metabolite could be detected in the urine of workers exposed to apparently low levels of MDI. Airborne MDI was sampled on 1-(2-methoxyphenyl)-piperazine (2MP)-impregnated glass fibre filters and determined by high-performance liquid chromatography (HPLC) using ultraviolet (UV) and electrochemical (EC) detection. The limit of detection of MDI was 3 ng ml-1 for a 20 microliters injection. The precision of sample preparation, expressed as relative standard deviation (RSD), was 1.3% with UV detection and 2.1% with EC detection at a concentration of 70 ng MDI ml-1 (n = 6). The 2MP-MDI derivative was stable at +4 degrees C up to eight weeks. The accuracy of the method was validated in an international quality control programme. Workers (n = 57) from three different factories participated in the study. Urinary 4,4'-methylenedianiline (MDA) metabolite was determined after acid hydrolysis as heptafluorobutyric anhydride derivatives by gas chromatography-mass spectrometry using chemical ionisation and monitoring negative ions. The limit of detection in urine was 0.2 nmol l-1. The precision of six analyses for a urine sample spiked to a concentration of 1 nmol l-1 was 29% (RSD). The MDI concentrations were below the limit of detection in most (64%) of the air samples collected in the worker's breathing zone. Still, detectable amounts of MDA were found in 97% of the urine samples. Monitoring of urinary MDA appears to be an appropriate method of assessing MDI exposure in work environments with low or undetectable MDI concentrations in the workplace air.
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Roman, Mark C
2013-01-01
A rapid method has been developed to quantify seven catechins and caffeine in green tea (Camillia sinensis) raw material and powdered extract, and dietary supplements containing green tea extract. The method utilizes RP HPLC with a phenyl-based stationary phase and gradient elution. Detection is by UV absorbance. The total run time, including column re-equilibration, is 13 min. Single-laboratory validation (SLV) has been performed on the method to determine the repeatability, accuracy, selectivity, LOD, LOQ, ruggedness, and linearity for (+)-catechin, (-)-epicatechin, (-)-epicatechin gallate, (-)-epigallocatechin, (-)-gallocatechin gallate, (-)-epigallocatechin gallate, and (+)-gallocatechin, as well as caffeine. Repeatability precision and recovery results met AOAC guidelines for SLV studies for all catechins and caffeine down to a level of approximately 20 mg/g. Finished products containing high concentrations of minerals require the use of EDTA to prevent decomposition of the catechins.
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Jeong, Birang; Roh, Jong Seong; Yoon, Michung; Yoon, Yoosik; Shin, Soon Shik; Cho, Hyun Joo; Kwon, Yong Soo; Yang, Heejung
2018-01-01
DF formula is a herbal preparation comprised three medicinal herbs, namely, Ephedra intermedia , Rheum palmatum , and Lithospermum erythrorhizon , which is being used for the treatment of obesity and liver fibrosis in Korean local clinics. Since the abovementioned three herbs exist with different proportions in DF formula and their chemical markers have different physiochemical properties; it is quite challenging to develop an analytical methodology for the determination of these chemical markers. For the analysis of the three herbs, five chemicals, (+)-pseudoephedrine (1) and (-)-ephedrine (2) for E. intermedia , aloe-emodin (3), and chrysophanol (4) for R. palmatum , and shikonin (5) for L. erythrorhizon , were selected for method validation of DF formula, and the analytical conditions were optimized and validated using high-performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). The specificities for the five compounds 1-5 were determined by their UV absorption spectra (1-4: 215 nm and 5: 520 nm). Their calibration curves showed good linear regressions with high correlation coefficient values ( R 2 > 0.9997). The limits of detection of these five markers were in the range 0.4-2.1 ng/mL, with the exception of 5 (12.7 ng/mL). The intraday variability for all the chemical markers was less than a Relative standard deviation (RSD) of 3%, except for 5 (RSD = 12.6%). In the case of interday analysis, 1 (1.0%), 2 (3.1%), and 4 (3.7%) showed much lower variabilities (RSD < 5%) than 3 (7.6%) and 5 (8.2%). Moreover, the five chemical markers showed good recoveries with good accuracies in the range of 90%-110%. The developed HPLC-UV method for the determination of the five chemical markers of the components of DF formula was validated. DF formula, the herbal composition of Ephedra intermedia , Rheum palmatum and Lithospermum erythrorhizon Five chemical markers in DF formula were (+)-pseudoephedrine (1) and (-)-ephedrine (2) for E. intermedia , aloe-emodin (3) and chrysopanol (4) for R. palmatum , and shikonin (5) for L. erythrorhizon , with quite different physico-chemical propertiesFive chemical markers in DF formula were determined by HPLC-UV Abbreviations used: EP: (-)-ephedrine; PSEP: (+)-pseudoephedrine; HPLC: High-performance liquid chromatography; UV: Ultraviolet; LOD: Limit of detection; LOQ: Limit of quantification; RSD: Relative standard deviation.
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USDA-ARS?s Scientific Manuscript database
A single laboratory validation has been performed on a practical ultra high-performance liquid chromatography (UHPLC), diode array detection (DAD), and tandem mass spectrometry (MS) method for determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved u...
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Hsieh, Han-Yun; Shyu, Ching-Lin; Liao, Chen-Wei; Lee, Ren-Jye; Lee, Maw-Rong; Vickroy, Thomas W; Chou, Chi-Chung
2012-04-01
Zeranol (Z) is a semi-synthetic mycotoxin that is used in some countries as a growth-promoting agent in livestock. In view of the known oestrogenic actions by Z and certain Z analogues, significant concerns exist with regard to the presence of Z residues in human foods and the potential for untoward effects, including carcinogenicity within the reproductive system. In order to confirm that foods are free from harmful Z residues, regulators need a quick and reliable analytical method that can be used for routine confirmation of Z-positive samples identified by enzyme-linked immunosorbent assay (ELISA) screening. In this study the authors have developed and validated a simple and rapid high-performance liquid chromatography method incorporating ultraviolet (UV) absorbance (wavelength 274 nm) and electrochemical (EC) dual-mode detection for simultaneous determination of Z-related mycotoxins produced from mouldy grain matrices, including rice, soybean and corn flakes. Recoveries for all analytes were around 80% and the limits of detection ranged from 10 to 25 ng mL(-1) for UV and from 50 to 90 ng mL(-1) for EC detection with good accuracy and reproducibility. Differential profiles and occurrence rates of Z, β-zearalenol, β-zearalanol and α-zearalenol in naturally moulded grain matrices were observed, indicating different metabolite patterns and possibly grain-specific effects of mycotoxin exposure for humans and animals. The strength of this dual detection method lies in its selectivity characterised by a carbon screen-printed electrode such that aflatoxin interference is precluded. The combined dual detection technique affords quick and reliable semi-confirmative and quantitative information on multiple types of Z analogues in mouldy grains without the necessity of using expensive mass spectrometry. The method is considered a superior supplement to ELISA, which only screens total Z immunoreactivity. Copyright © 2011 Society of Chemical Industry.
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Qi, Xiaoquan; Bakht, Saleha; Devos, Katrien M.; Gale, Mike D.; Osbourn, Anne
2001-01-01
A flexible, non-gel-based single nucleotide polymorphism (SNP) detection method is described. The method adopts thermostable ligation for allele discrimination and rolling circle amplification (RCA) for signal enhancement. Clear allelic discrimination was achieved after staining of the final reaction mixtures with Cybr-Gold and visualisation by UV illumination. The use of a compatible buffer system for all enzymes allows the reaction to be initiated and detected in the same tube or microplate well, so that the experiment can be scaled up easily for high-throughput detection. Only a small amount of DNA (i.e. 50 ng) is required per assay, and use of carefully designed short padlock probes coupled with generic primers and probes make the SNP detection cost effective. Biallelic assay by hybridisation of the RCA products with fluorescence dye-labelled probes is demonstrated, indicating that ligation-RCA (L-RCA) has potential for multiplexed assays. PMID:11713336
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NASA Astrophysics Data System (ADS)
Beegle, L. W.; Bhartia, R.; DeFlores, L. P.; Abbey, W.; Asher, S. A.; Burton, A. S.; Fries, M.; Conrad, P. G.; Clegg, S. M.; Wiens, R. C.; Edgett, K. S.; Ehlmann, B. L.; Nealson, K. H.; Minitti, M. E.; Popp, J.; Langenhorst, F.; Sobron, P.; Steele, A.; Williford, K. H.; Yingst, R. A.
2017-12-01
The Scanning Habitable Environments with Raman & Luminescence for Organics & Chemicals (SHERLOC) investigation is part of the Mars 2020 integrated payload. SHERLOC enables non-contact, spatially resolved, and highly sensitivity detection and characterization of organics and minerals in the Martian surface and near subsurface. SHERLOC is an arm-mounted, Deep UV (DUV) resonance Raman and fluorescence spectrometer utilizing a 248.6-nm DUV laser. Deep UV induced native fluorescence is very sensitive to condensed carbon and aromatic organics, enabling detection at or below 10-6 w/w (1 ppm) at <100 µm spatial scales. SHERLOC's deep UV resonance Raman enables detection and classification of aromatic and aliphatic organics with sensitivities of 10-2 to below 10-4 w/w. In addition to organics, the deep UV Raman enables detection and classification of minerals relevant to aqueous chemistry with grain sizes below 20 µm. SHERLOC will be able to map the distribution of organic material with respect to visible features and minerals that are identifiable with the Raman spectrometer. These maps will enable analysis of the distribution of organics with minerals.
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Design of the NDUV detection circuit for the NO concentration of the vehicle exhaust emissions
NASA Astrophysics Data System (ADS)
Zhang, Kai; Zhang, Yujun; He, Ying; You, Kun; Gao, Yanwei; Chen, Chen; Liu, Guohua; He, Chungui; Lu, Yibing; Liu, Wenqing
2016-10-01
With the increasing number of vehicles, the harm from NO to the environment becomes more and more prominent. So the monitoring of the NO concentration of the vehicle exhaust emissions is very important to assess the emission levels. In this paper, the NO detection system designing for vehicle exhaust emissions based on the non-dispersive ultraviolet principle (NDUV) has been researched. The technical indexes of the two-way modulation UV signal detection circuit are discussed in detail. And then a precision detection circuit is designed, which is composed of a trans-impedance amplifier and a lock-in amplifier, with which the output of the UV photoelectric detector can be amplified to a suitable voltage range, and the DC noise of the pre-stage amplifier is effectively removed by the lock-in amplifier. An experimental system was set up to test the designed circuit. To ensure the consistency of the two channels, the method of exchange calibration was adopted in the test. It's drawn that the designed circuit is of high SNR, measuring accuracy and a large dynamic range from the test results. The NO concentration detection limit of vehicle emissions can reach 1ppm, and the detection precision is +/-15ppm.
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Single-strand breakage of DNA in UV-irradiated uvrA, uvrB, and uvrC mutants of Escherichia coli.
Tang, M S; Ross, L
1985-01-01
We transduced the uvrA6, uvrB5, uvrC34, and uvrC56 markers from the original mutagenized strains into an HF4714 background. Although in the original mutagenized strains uvrA6 cells are more UV sensitive than uvrB5 and uvrC34 cells, in the new background no significant difference in UV sensitivity is observed among uvrA6, uvrB5, and uvrC34 cells. No DNA single-strand breaks are detected in UV-irradiated uvrA6 or uvrB5 cells, whereas in contrast a significant number of single-strand breaks are detected in both UV-irradiated uvrC34 and uvrC56 cells. The number of single-strand breaks in these cells reaches a plateau at 20-J/m2 irradiation. Since these single-strand breaks can be detected by both alkaline sucrose and neutral formamide-sucrose gradient sedimentation, we concluded that the single-strand breaks observed in UV-irradiated uvrC cells are due to phosphodiester bond interruptions in DNA and are not due to apurinic/apyrimidinic sites. PMID:3882671
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Wu, Ming-Hong; Li, Jian; Xu, Gang; Ma, Luo-Dan; Li, Jia-Jun; Li, Jin-Song; Tang, Liang
2018-05-15
The environmental behaviors of emerging pollutants, benzophenone-type UV filters (BP-UV filters) and their derivatives were investigated in four wastewater treatment plants (WWTPs), and their receiving surface waters in Shanghai. The concentration level of selected BP-UV filters in the WWTPs was detected from ngL -1 to μgL -1 . BP (621-951ngL -1 ) and BP-3 (841-1.32 × 10 3 ngL -1 ) were the most abundant and highest detection frequency individuals among the target BP-UV filters in influents, whereas BP (198-400ngL -1 ), BP-4 (93.3-288ngL -1 ) and BP-3 (146-258ngL -1 ) were predominant in effluents. BP-UV filters cannot be completely removed and the total removal efficiency varied widely (-456% to 100%) during the treatment process. It can be inferred that the usage of BP and BP-3 are higher than other BP-UV filters in the study area. The lowest and highest levels were BP-2 (ND-7.66ngL -1 ) and BP-3 (68.5-5.01 × 10 3 ng L -1 ) in the receiving surface water, respectively. Interestingly, the seasonal variation of BP-3 is larger than those of other BP-UV filters in surface water from Shanghai. There is no obvious pollution pattern of BP-UV filters in the surface water from the cosmetic factory area. The correlation analysis of BP-UV filters between WWTPs effluents and nearby downstream water samples suggested that BP-UV filters emitted from some WWTPs might be the main source of receiving surface water. Preliminary risk assessment indicated that the levels of BP-UV filters detected by the effluent posed medium to high risk to fish as well as other aquatic organisms. Copyright © 2018 Elsevier Inc. All rights reserved.
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NASA Astrophysics Data System (ADS)
Wang, Zhiyuan
Solar-blind ultraviolet detection refers to photon detection specifically in the wavelength range of 200 nm to 320 nm. Without background noises from solar radiation, it has broad applications from homeland security to environmental monitoring. In this thesis, we design and fabricate a nanophotonic metal-oxide-semiconductor device for solar-blind UV detection. Instead of using semiconductors as the active absorber, we use metal Sn nano- grating structures to absorb UV photons and generate hot electrons for internal photoemission across the Sn/SiO 2 interfacial barrier, thereby generating photocurrent between metal and semiconductor region upon UV excitation. The large metal/oxide interfacial energy barrier enables solar-blind UV detection by blocking the less energetic electrons excited by visible photons. With optimized design, 85% UV absorption and hot electron excitation can be achieved within the mean free path of 20 nm from the metal/oxide interface. This feature greatly enhances hot electron transport across the interfacial barrier to generate photocurrent. Various fabrication techniques have been developed for preparing nano gratings. For nominally 20 nm-thick deposited Sn, the self- formed pseudo-periodic nanostructure help achieve 75% UV absorption from lambda=200 nm to 300 nm. With another layer of nominally 20 nm-thick Sn, similar UV absorption is maintained while conductivity is improved, which is beneficial for overall device efficiency. The Sn/SiO2/Si MOS devices show good solar-blind character while achieving 13% internal quantum efficiency for 260 nm UV with only 20 nm-thick Sn and some devices demonstrate much higher (even >100%) internal quantum efficiency. While a more accurate estimation of device effective area is needed for proving our calculation, these results indeed show a great potential for this type of hot-electron-based photodetectors and for Sn nanostructure as an effective UV absorber. The simple geometry of the self- assembled Sn nano-gratings and MOS structure make this novel type of device easy to fabricate and integrate with Si ROICs compared to existing solar-blind UV detection schemes. The presented device structure also breaks through the conventional notion that photon absorption by metal is always a loss in solid-state photodetectors, and it can potentially be extended to other active metal photonic devices.
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Choo, K S; Kim, I W; Jung, J K; Suh, Y G; Chung, S J; Lee, M H; Shim, C K
2001-06-01
A simple, reliable HPLC-UV detection method was developed for the simultaneous determination of loxoprofen and its metabolites (i.e. trans- and cis-alcohol metabolites), in human plasma and urine samples. The method involves the addition of a ketoprofen (internal standard) solution in methanol, zinc sulfate solution and acetonitrile to plasma and urine samples, followed by centrifugation. An aliquot of the supernatant was evaporated to dryness, and the residue reconstituted in a mobile phase (acetonitrile:water=35:65 v/v, pH 3.0). An aliquot of the solution was then directly injected into the HPLC system. Separations were performed on octadecylsilica column (250x4.5 mm, 5 microm) with a guard column (3.2x1.5 cm, 7 microm) at ambient temperature. Loxoprofen and the metabolites in the eluent were monitored at 220 nm (a.u.f.s. 0.005). Coefficients of variations (CV%) and recoveries for loxoprofen and its metabolites were below 10 and over 96%, respectively, in the 200 approximately 15000 ng ml(-1) range for plasma and 500 approximately 50000 ng ml(-1) range for urine. Calibration curves for all the compounds in the plasma and urine were linear over the above-mentioned concentration ranges with a common correlation coefficient of 0.999. The detection limit of the present method was 100 ng for all the compounds. These results indicate that the present method is very simple and readily applicable to routine bioavailability studies of these compounds with an acceptable sensitivity.
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Differential responses to high- and low-dose ultraviolet-B stress in tobacco Bright Yellow-2 cells
Takahashi, Shinya; Kojo, Kei H.; Kutsuna, Natsumaro; Endo, Masaki; Toki, Seiichi; Isoda, Hiroko; Hasezawa, Seiichiro
2015-01-01
Ultraviolet (UV)-B irradiation leads to DNA damage, cell cycle arrest, growth inhibition, and cell death. To evaluate the UV-B stress–induced changes in plant cells, we developed a model system based on tobacco Bright Yellow-2 (BY-2) cells. Both low-dose UV-B (low UV-B: 740 J m−2) and high-dose UV-B (high UV-B: 2960 J m−2) inhibited cell proliferation and induced cell death; these effects were more pronounced at high UV-B. Flow cytometry showed cell cycle arrest within 1 day after UV-B irradiation; neither low- nor high-UV-B–irradiated cells entered mitosis within 12 h. Cell cycle progression was gradually restored in low-UV-B–irradiated cells but not in high-UV-B–irradiated cells. UV-A irradiation, which activates cyclobutane pyrimidine dimer (CPD) photolyase, reduced inhibition of cell proliferation by low but not high UV-B and suppressed high-UV-B–induced cell death. UV-B induced CPD formation in a dose-dependent manner. The amounts of CPDs decreased gradually within 3 days in low-UV-B–irradiated cells, but remained elevated after 3 days in high-UV-B–irradiated cells. Low UV-B slightly increased the number of DNA single-strand breaks detected by the comet assay at 1 day after irradiation, and then decreased at 2 and 3 days after irradiation. High UV-B increased DNA fragmentation detected by the terminal deoxynucleotidyl transferase dUTP nick end labeling assay 1 and 3 days after irradiation. Caffeine, an inhibitor of ataxia telangiectasia mutated (ATM) and ataxia telangiectasia and Rad3-related (ATR) checkpoint kinases, reduced the rate of cell death in high-UV-B–irradiated cells. Our data suggest that low-UV-B–induced CPDs and/or DNA strand-breaks inhibit DNA replication and proliferation of BY-2 cells, whereas larger contents of high-UV-B–induced CPDs and/or DNA strand-breaks lead to cell death. PMID:25954287
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NASA Astrophysics Data System (ADS)
Hug, W. F.; Reid, R. D.; Bhartia, R.; Lane, A. L.
2008-04-01
Improvised explosive devices (IEDs), vehicle-borne improvised explosive devices (VBIEDs), and suicide bombers are a major threat to many countries and their citizenry. The ability to detect trace levels of these threats with a miniature, hand-held, reagentless, standoff sensor represents a major improvement in the state of the art of CBE surface sensors. Photon Systems, Inc., in collaboration with Jet Propulsion Laboratory, recently demonstrated a new technology hand-held sensor for reagentless, close-range, standoff detection and identification of trace levels CBE materials on surfaces. This targeted ultraviolet CBE (TUCBE) sensor is the result of an Army Phase I STTR program. The resulting 5lb, 5W, flashlight-sized sensor can discriminate CBE from background materials using a combination of deep UV excited resonance Raman (RR) and laser induced native fluorescence (LINF) emissions resulting from excitation by a new technology deep UV laser. Detection and identification is accomplished in less than 1ms. Standoff excitation of suspicious packages, vehicles, persons, and other objects that may contain hazardous materials is accomplished using wavelengths below 250nm where Raman and native fluorescence emissions occupy distinctly different wavelength regions. This enables simultaneous detection of RR and LINF emissions with no interferences. The sensor employs fused RR/LINF chemometric methods to extract the identity of targeted materials from background clutter. Photon Systems has demonstrated detection and identification of 100ng/cm2 of explosives materials at a distance of 1 meter using a sensor with 3.8 cm optical aperture. Expansion of the optical aperture to 38 cm in a lantern-sized sensor will enable similar detection and identification of CBE materials at standoff distances of 10 meters. As a result of excitation and detection in the deep UV and the use of a gated detection system, the sensor is solar blind and can operate in full daylight conditions.
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Lavigne, Claire; Durand, Gérard; Roblin, Antoine
2006-12-20
Light scattering in the atmosphere by particles and molecules gives rise to an aureole surrounding the source image that tends to reduce the contrast of the source with respect to the background. However, UV scattering phase functions of the haze droplets present a very important forward peak. The spreading of a detected signal in the UV is not as important as in the case of a clear atmosphere where Rayleigh scattering predominates. This physical property has to be taken into account to evaluate the potential of UV radiation as an aircraft landing aid under low visibility conditions. Different results characterizing UV runway lights, simulations of UV radiation propagation in the atmosphere, and the use of a simple detection algorithm applied to one particular sensor are presented.
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Gilmartin, Gregory; Gingrich, Diane
2018-04-15
The determination and speciation of arsenic in natural resources such as drinking water and agricultural soils has been a growing concern in recent years due to its many toxicological effects [1-3]. To speciate and quantitate concentrations of <1 ppm of arsenic, typically an ion chromatograph (IC) interfaced to an inductively coupled plasma mass spectrometer (ICP-MS) is employed [4-9]. This methodology may be very robust and sensitive, but it is expensive and not as ubiquitous as high performance liquid chromatography (HPLC) with ultraviolet (UV) absorbance detection or electrospray ionization mass spectrometry (ESI-MS). Anion exchange chromatography is a well-documented means of speciating arsenite (As(III), As 2 O 3 ) and arsenate (As(V), AsO 4 ) using UV [10], conductivity [11], or ESI-MS detection [12,13]. This paper demonstrates the utilization of common liquid chromatographic instrumentation to speciate and determines inorganic Arsenic compounds using UV or MS via selected ion recording (SIR) or multiple reaction monitoring (MRM) detection. This paper describes the analysis of arsenite and arsenate samples prepared using both deionized and ground water. The limit of quantitation for the techniques described in this paper for samples spiked in ground water were 454 ppb (As(III)) and 562 ppb (As(V)) for UV detection, 45.4 ppb (As(III)) and 56.2 ppb (As(V)) for SIR detection, and 4.54 ppb (As(III)) and 5.62 ppb (As(V)) for MRM detection. Copyright © 2018 Elsevier B.V. All rights reserved.
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Fluorescence-Assisted Gamma Spectrometry for Surface Contamination Analysis
NASA Astrophysics Data System (ADS)
Ihantola, Sakari; Sand, Johan; Perajarvi, Kari; Toivonen, Juha; Toivonen, Harri
2013-02-01
A fluorescence-based alpha-gamma coincidence spectrometry approach has been developed for the analysis of alpha-emitting radionuclides. The thermalization of alpha particles in air produces UV light, which in turn can be detected over long distances. The simultaneous detection of UV and gamma photons allows detailed gamma analyses of a single spot of interest even in highly active surroundings. Alpha particles can also be detected indirectly from samples inside sealed plastic bags, which minimizes the risk of cross-contamination. The position-sensitive alpha-UV-gamma coincidence technique reveals the presence of alpha emitters and identifies the nuclides ten times faster than conventional gamma spectrometry.
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Yılmaz, Pelin Köseoğlu; Ertaş, Abdulselam; Kolak, Ufuk
2014-08-01
A sensitive, rapid, and simple high-performance liquid chromatography with UV detection method was developed for the simultaneous determination of seven phthalic acid esters (dimethyl phthalate, dipropyl phthalate, di-n-butyl phthalate, benzyl butyl phthalate, dicyclohexyl phthalate, di-(2-ethylhexyl) phthalate, and di-n-octyl phthalate) in several kinds of beverage samples. Ultrasound and vortex-assisted dispersive liquid-liquid microextraction method was used. The separation was performed using an Intersil ODS-3 column (C18 , 250 × 4.6 mm, 5.0 μm) and a gradient elution with a mobile phase consisting of MeOH/ACN (50:50) and 0.2 M KH2 PO4 buffer. Analytes were detected by a UV detector at 230 nm. The developed method was validated in terms of linearity, limit of detection, limit of quantification, repeatability, accuracy, and recovery. Calibration equations and correlation coefficients (> 0.99) were calculated by least squares method with weighting factor. The limit of detection and quantification were in the range of 0.019-0.208 and 0.072-0.483 μg/L. The repeatability and intermediate precision were determined in terms of relative standard deviation to be within 0.03-3.93 and 0.02-4.74%, respectively. The accuracy was found to be in the range of -14.55 to 15.57% in terms of relative error. Seventeen different beverage samples in plastic bottles were successfully analyzed, and ten of them were found to be contaminated by different phthalic acid esters. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Shkolyar, Svetlana; Eshelman, Evan J; Farmer, Jack D; Hamilton, David; Daly, Michael G; Youngbull, Cody
2018-04-01
The Mars 2020 mission will analyze samples in situ and identify any that could have preserved biosignatures in ancient habitable environments for later return to Earth. Highest priority targeted samples include aqueously formed sedimentary lithologies. On Earth, such lithologies can contain fossil biosignatures as aromatic carbon (kerogen). In this study, we analyzed nonextracted kerogen in a diverse suite of natural, complex samples using colocated UV excitation (266 nm) time-gated (UV-TG) Raman and laser-induced fluorescence spectroscopies. We interrogated kerogen and its host matrix in samples to (1) explore the capabilities of UV-TG Raman and fluorescence spectroscopies for detecting kerogen in high-priority targets in the search for possible biosignatures on Mars; (2) assess the effectiveness of time gating and UV laser wavelength in reducing fluorescence in Raman spectra; and (3) identify sample-specific issues that could challenge rover-based identifications of kerogen using UV-TG Raman spectroscopy. We found that ungated UV Raman spectroscopy is suited to identify diagnostic kerogen Raman bands without interfering fluorescence and that UV fluorescence spectroscopy is suited to identify kerogen. These results highlight the value of combining colocated Raman and fluorescence spectroscopies, similar to those obtainable by SHERLOC on Mars 2020, to strengthen the confidence of kerogen detection as a potential biosignature in complex natural samples. Key Words: Raman spectroscopy-Laser-induced fluorescence spectroscopy-Mars Sample Return-Mars 2020 mission-Kerogen-Biosignatures. Astrobiology 18, 431-453.
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Tsui, Mirabelle M P; Leung, H W; Lam, Paul K S; Murphy, Margaret B
2014-04-15
Organic ultraviolet (UV) filters are applied widely in personal care products (PCPs), but the distribution and risks of these compounds in the marine environment are not well known. In this study, the occurrence and removal efficiencies of 12 organic UV filters in five wastewater treatment plants (WWTPs) equipped with different treatment levels in Hong Kong, South China, were investigated during one year and a preliminary environmental risk assessment was carried out. Using a newly developed simultaneous multiclass quantification liquid chromatography-tandem mass spectrometry (LC-MS/MS) method, butyl methoxydibenzoylmethane (BMDM), 2,4-dihydroxybenzophenone (BP-1), benzophenone-3 (BP-3), benzophenone-4 (BP-4) and 2-ethyl-hexyl-4-trimethoxycinnamate (EHMC) were frequently (≥80%) detected in both influent and effluent with mean concentrations ranging from 23 to 1290 ng/L and 18-1018 ng/L, respectively; less than 2% of samples contained levels greater than 1000 ng/L. Higher concentrations of these frequently detected compounds were found during the wet/summer season, except for BP-4, which was the most abundant compound detected in all samples in terms of total mass. The target compounds behaved differently depending on the treatment level in WWTPs; overall, removal efficiencies were greater after secondary treatment when compared to primary treatment with >55% and <20% of compounds showing high removal (defined as >70% removal), respectively. Reverse osmosis was found to effectively eliminate UV filters from effluent (>99% removal). A preliminary risk assessment indicated that BP-3 and EHMC discharged from WWTPs may pose high risk to fishes in the local environment. Copyright © 2014 Elsevier Ltd. All rights reserved.
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Wang, Yanfang; Yang, Na; Liu, Yi
2018-04-05
A novel organic small molecule with D-Pi-A structure was prepared, which was found to be a promising colorimetric and ratiometric UV-vis spetral probe for detection of phosphorylated proteins with the help of tetravalent zirconium ion. Such optical probe based on chromophore WYF-1 shows a rapid response (within 10s) and high selectivity and sensitivity for phosphorylated proteins, giving distinct colorimetric and ratiometric UV-vis changes at 720 and 560nm. The detection limit for phosphorylated proteins was estimated to be 100nM. In addition, detection of phosphorylated proteins in placental tissue samples with this probe was successfully applied, which indicates that this probe holds great potential for phosphorylated proteins detection. Copyright © 2018 Elsevier B.V. All rights reserved.
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Chaparro, L L; Ferrer, L; Cerdà, V; Leal, L O
2012-09-01
A multisyringe flow-injection approach has been coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS) with UV photo-oxidation for dimethylarsinic (DMA), inorganic As and total As determination, depending on the pre-treatment given to the sample (extraction or digestion). The implementation of a UV lamp allows on-line photo-oxidation of DMA and the following arsenic detection, whereas a bypass leads the flow directly to the HG-AFS system, performing inorganic arsenic determination. DMA concentration is calculated by the difference of total inorganic arsenic and measurement of the photo-oxidation step. The detection limits for DMA and inorganic arsenic were 0.09 and 0.47 μg L(-1), respectively. The repeatability values accomplished were of 2.4 and 1.8%, whereas the injection frequencies were 24 and 28 injections per hour for DMA and inorganic arsenic, respectively. This method was validated by means of a solid reference material BCR-627 (muscle of tuna) with good agreement with the certified values. Satisfactory results for DMA and inorganic arsenic determination were obtained in several water matrices. The proposed method offers several advantages, such as increasing the sampling frequency, low detection limits and decreasing reagents and sample consumption, which leads to lower waste generation.
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Colorimetric detection of DNA damage by using hemin-graphene nanocomposites
NASA Astrophysics Data System (ADS)
Wei, W.; Zhang, D. M.; Yin, L. H.; Pu, Y. P.; Liu, S. Q.
2013-04-01
A colorimetric method for detection of DNA damage was developed by using hemin-graphene nanosheets (H-GNs). H-GNs were skillfully synthesized by adsorping of hemin on graphene through π-π interactions. The as-prepared H-GNs possessed both the ability of graphene to differentiate the damage DNA from intact DNA and the catalytic action of hemin. The damaged DNA made H-GNs coagulated to different degrees from the intact DNA because there were different amount of negative charge exposed on their surface, which made a great impact on the solubility of H-GNs. As a result, the corresponding centrifugal supernatant of H-GNs solution showed different color in the presence of 3,3',5,5'-tetramethylbenzidine (TMB) and H2O2, which could be discriminated by naked eyes or by ultraviolet (UV)-visible spectrometer. Based on this, the damaged effects of styrene oxide (SO), NaAsO2 and UV radiation on DNA were studied. Results showed that SO exerted most serious damage effect on DNA although all of them damaged DNA seriously. The new method for detection of DNA damage showed good prospect in the evaluation of genotoxicity of new compounds, the maximum limit of pesticide residue, food additives, and so on, which is important in the fields of food science, pharmaceutical science and pesticide science.
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Qu, Jialin; Gong, Tianxing; Ma, Bin; Zhang, Lin; Kano, Yoshihiro; Yuan, Dan
2012-01-01
The purpose of the study is to compare alkaloid profile of Uncaria rhynchophylla hooks and leaves. Ten oxindole alkaloids and four glycosidic indole alkaloids were identified using HPLC-diode array detection (DAD) or LC-atmospheric pressure chemical ionization (APCI)-MS method, and a HPLC-UV method for simultaneous quantification of major alkaloids was validated. The hooks are characterized by high levels of four oxindole alkaloids rhynchophylline (R), isorhynchophylline (IR), corynoxeine (C) and isocorynoxeine (IC), while the leaves contained high level of two glycosidic indole alkaloids vincoside lactam (VL) and strictosidine (S). The presented methods have proven its usefulness in chemical characterization of U. rhynchophylla hooks and leaves.
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NASA Astrophysics Data System (ADS)
Fornaro, T.; Brucato, J. R.; ten Kate, I. L.; Siljeström, S.; Steele, A.; Cody, G. D.; Hazen, R. M.
2018-04-01
We present laboratory activities of preparation, characterization, and UV irradiation processing of Mars soil analogues, which are key to support both in situ exploration and sample return missions devoted to detection of molecular biomarkers on Mars.
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Indium nanoparticles for ultraviolet surface-enhanced Raman spectroscopy
NASA Astrophysics Data System (ADS)
Das, Rupali; Soni, R. K.
2018-05-01
Ultraviolet Surface-enhanced Raman spectroscopy (UVSERS) has emerged as an efficient molecular spectroscopy technique for ultra-sensitive and ultra-low detection of analyte concentration. The generic SERS substrates based on gold and silver nanostructures have been extensively explored for high local electric field enhancement only in visible-NIR region of the electromagnetic spectrum. The template synthesis of controlled nanoscale size metallic nanostructures supporting localized surface plasmon resonance (LSPR) in the UV region have been recently explored due to their ease of synthesis and potential applications in optoelectronic, catalysis and magnetism. Indium (In0) nanoparticles exhibit active surface plasmon resonance (SPR) in ultraviolet (UV) and deep-ultaviolet (DUV) region with optimal absorption losses. This extended accessibility makes indium a promising material for UV plasmonic, chemical sensing and more recently in UV-SERS. In this work, spherical indium nanoparticles (In NPs) were synthesized by modified polyol reduction method using NaBH4 having local surface plasmon resonance near 280 nm. The as-synthesized spherical In0 nanoparticles were then coated with thin silica shells of thickness ˜ 5nm by a modified Stober method protecting the nanoparticles from agglomeration, direct contact with the probed molecules as well as prevent oxidation of the nanoparticles. Morphological evolution of In0 nanoparticles and SiO2 coating were characterized by transmission electron microscope (TEM). An enhanced near resonant shell-isolated SERS activity from thin film of tryptophan (Tryp) molecules deposited on indium coated substrates under 325nm UV excitation was observed. Finite difference time domain (FDTD) method is employed to comprehend the experimental results and simulate the electric field contours which showed amplified electromagnetic field localized around the nanostructures. The comprehensive analysis indicates that indium is a promising alternate exogenous contrast agent for efficient Raman spectroscopy from molecules.
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Olsson, Petter; Holmbäck, Jan; Herslöf, Bengt
2014-11-21
This paper reports a simple chromatographic system to separate lipids classes as well as their molecular species. By the use of phenyl coated silica as stationary phase in combination with a simple mobile phase consisting of methanol and water, all tested lipid classes elute within 30 min. Furthermore, a method to accurately predict retention times of specific lipid components for this type of chromatography is presented. Common detection systems were used, namely evaporative light scattering detection (ELSD), charged aerosol detection (CAD), electrospray mass spectrometry (ESI-MS), and UV detection. Copyright © 2014 Elsevier B.V. All rights reserved.
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Taraji, Maryam; Talebpour, Zahra; Adib, Nuoshin; Karimi, Shima; Haghighi, Farideh; Aboul-Enein, Hassan Y
2015-09-01
A sensitive, selective and simple method for the simultaneous determination of carvedilol enantiomers in aqueous solution has been developed using stir bar sorptive extraction (SBSE) followed by high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection. This method is based on the reaction of carvedilol enantiomers with (-)-menthyl chloroformate (MCF) after extraction by the SBSE method to produce diastereomeric derivatives. The separation was achieved by use of a C18 analytical column and the influence of mobile phase composition on the enantioseparation of carvedilol was studied. The applicability of two sorptive phases, poly(methyl methacrylate/ethyleneglycol dimethacrylate) (PA-EG) and polydimethylsiloxane, were tested for extraction of carvedilol enantiomers from aqueous samples. The obtained results showed excellent linear dynamic ranges and precisions for each of them. The least limit of detection for (S)- and (R)-carvedilol obtained 8 and 11 µg L(-1), respectively, using the PA-EG sorptive phase. Inter- and intra-mean recoveries were also satisfactory, ranging from 98 to 103%, with coefficient of variation in the range of 1-5% at three fortified levels using a PA-EG coated stir bar. The proposed SBSE (PA-EG)-MCF derivatization-HPLC-UV method was successfully applied to enantioselective analysis of carvedilol in water and pharmaceutical dosages, confirming the application of this method. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
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The repair of low dose UV light-induced damage to human skin DNA in condition of trace amount Mg 2+
NASA Astrophysics Data System (ADS)
Gao, Fang; Guo, Zhouyi; Zheng, Changchun; Wang, Rui; Liu, Zhiming; Meng, Pei; Zhai, Juan
2008-12-01
Ultraviolet light-induced damage to human skin DNA was widely investigated. The primary mechanism of this damage contributed to form cyclobutane pyrimidine dimmers (CPDs). Although the distribution of UV light-induced CPDs within a defined sequence is similar, the damage in cellular environment which shields the nuclear DNA was higher than that in organism in apparent dose. So we use low UVB light as main study agent. Low dose UV-irradiated HDF-a cells (Human Dermal Fibroblasts-adult cells) which is weaker than epidermic cells were cultured with DMEM at different trace amount of Mg2+ (0mmol/L , 0.1mmol/L , 0.2mmol/L, 0.4mmol/L, 0.8mmol/L, 1.2mmol/L) free-serum DMEM and the repair of DNA strands injured were observed. Treat these cells with DNA strand breaks detection, photoproducts detection and the repair of photoproducts detection. Then quantitate the role of trace amount Mg2+ in repair of UV light-induced damage to human skin. The experiment results indicated that epidermic cells have capability of resistance to UV-radiation at a certain extent. And Mg2+ can regulate the UV-induced damage repair and relative vitality. It can offer a rationale and experiment data to relieve UV light-induced skin disease.
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2009-01-01
transient was present. BASELINE EXPERIMENT Methods Participants Sixteen young adults (9 women , 7 men ) aged 18–26 years (mean = 20.5) partic- ipated...Sixteen young adults (8 women , 8 men ) aged 18–28 years (mean = 21.9) partici- pated. The experiment lasted approximately 2 hours and participants were...based on the operator’s change detection performance. Mis- sion scenarios involved supervision of multiple UVs and required multitasking . Effects of
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Chan, W; Gerhardt, G C; Salisbury, C D
1994-01-01
A method for the simultaneous determination of tylosin and tilmicosin residues in animal tissues is reported. Solid-phase extraction columns are used to isolate the drugs from tissue extracts. Determination is accomplished by reversed-phase liquid chromatography with UV detection at 287 nm. Mean recoveries from spiked tissues were 79.9% (coefficient of variation [CV], 8.1%) for tylosin and 92.6% (CV, 8.7%) for tilmicosin. Detection limits for tylosin and tilmicosin were 0.020 and 0.010 ppm, respectively.
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Kim, Ki-Hyun; Szulejko, Jan E.; Kim, Yong-Hyun; Lee, Min-Hee
2014-01-01
The relative performance figure of merits was investigated for the two most common analytical methods employed for carbonyl compounds (CC), for example, between high performance liquid chromatography (HPLC)-UV detector (with 2,4-dinitrophenylhydrazine (DNPH) derivatization) and thermal desorption (TD)-gas chromatography (GC)-mass spectrometry (MS) (without derivatization). To this end, the suitability of each method is assessed by computing the relative recovery (RR) between the gas- and liquid-phase standards containing a suite of CC such as formaldehyde (FA), acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA) along with benzene (B) as a recovery reference for the GC method. The results confirm that a TD-GC-MS is advantageous to attain the maximum recovery for the heavier CCs (i.e., with molecular weights (MW) above BA−MW ≥ 74). On the other hand, the HPLC-UV is favorable for the lighter CCs (like FA and AA) with the least bias. Such compound-specific responses for each platform are validated by relative ordering of CCs as a function of response factor (RF), method detection limit (MDL), and recovery pattern. It is thus desirable to understand the advantages and limitations of each method to attain the CC data with the least experimental bias. PMID:24719571
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Kishikawa, Naoya; Kondo, Naoko; Amponsaa-Karikari, Abena; Kodamatani, Hitoshi; Ohyama, Kaname; Nakashima, Kenichiro; Yamazaki, Shigeo; Kuroda, Naotaka
2014-02-01
Isoamyl nitrite is used as a therapeutic reagent for cardiac angina and as an antidote for cyanide poisoning, but it is abused because of its euphoric properties. Therefore, a method to determine isoamyl nitrite is required in many fields, including pharmaceutical and forensic studies. In this study, a simple, rapid and sensitive method for the determination of isoamyl nitrite was developed using a flow injection analysis system equipped with a chemiluminescence detector and on-line photoreactor. This method is based on on-line ultraviolet irradiation of isoamyl nitrite and subsequent luminol chemiluminescence detection without the addition of an oxidant. A linear standard curve was obtained up to 1.0 μM of isoamyl nitrite with a detection limit (blank + 3SD) of 0.03 μM. The method was successfully applied to determine isoamyl nitrite content in pharmaceutical preparations. Copyright © 2013 John Wiley & Sons, Ltd.
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Xia, Zhenyang; Zang, Kai; Liu, Dong; ...
2017-08-21
Photo detection of ultraviolet (UV) light remains a challenge since the penetration depth of UV light is limited to the nanometer scale. Therefore, the doping profile and electric field in the top nanometer range of the photo detection devices become critical. Traditional UV photodetectors usually use a constant doping profile near the semiconductor surface, resulting in a negligible electric field, which limits the photo-generated carrier collection efficiency of the photodetector. Here, we demonstrate, via the use of an optimized gradient boron doping technique, that the carrier collection efficiency and photo responsivity under the UV wavelength region have been enhanced. Moreover,more » the ultrathin p+-i-n junction shows an avalanche gain of 2800 and an ultra-low junction capacitance (sub pico-farad), indicating potential applications in the low timing jitter single photon detection area.« less
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Xia, Zhenyang; Zang, Kai; Liu, Dong
Photo detection of ultraviolet (UV) light remains a challenge since the penetration depth of UV light is limited to the nanometer scale. Therefore, the doping profile and electric field in the top nanometer range of the photo detection devices become critical. Traditional UV photodetectors usually use a constant doping profile near the semiconductor surface, resulting in a negligible electric field, which limits the photo-generated carrier collection efficiency of the photodetector. Here, we demonstrate, via the use of an optimized gradient boron doping technique, that the carrier collection efficiency and photo responsivity under the UV wavelength region have been enhanced. Moreover,more » the ultrathin p+-i-n junction shows an avalanche gain of 2800 and an ultra-low junction capacitance (sub pico-farad), indicating potential applications in the low timing jitter single photon detection area.« less
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A new rhodamine-based colorimetric chemosensor for naked-eye detection of Cu2 + in aqueous solution
NASA Astrophysics Data System (ADS)
Hu, Yang; Zhang, Jing; Lv, Yuan-Zheng; Huang, Xiao-Huan; Hu, Sheng-li
2016-03-01
A new colorimetric probe 1 based on rhodamine B lactam was developed for naked-eye detection of Cu2 +. The optical feature of 1 for Cu2 + was investigated by UV-vis absorption spectroscopy. Upon the addition of Cu2 +, the 1 displayed a distinct color change from colorless to pink, which can be directly detected by the naked eye. The stoichiometry of 1 to Cu2 + complex was found to be 1:1 and the naked-eye detection limit was determined as low as 2 μM. The results suggest that the probe 1 may provide a convenient method for visual detection of Cu2 + with high sensitivity.
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An HPLC method for determination of azadirachtin residues in bovine muscle.
Gai, María Nella; Álvarez, Christian; Venegas, Raúl; Morales, Javier
2011-04-01
A high-performance liquid chromatography (HPLC) method for the determination of azadirachtin (A and B) residues in bovine muscle has been developed. Azadirachtin is a neutral triterpene and chemotherapeutic agent effective in controlling some pest flies in horses, stables, horns and fruit. The actual HPLC method uses an isocratic elution and UV detection. Liquid-liquid extraction and solid-phase purification was used for the clean-up of the biological matrix. The chromatographic determination of these components is achieved using a C18 analytical column with water-acetonitrile mixture (27.5:72.5, v/v) as mobile phase, 1 mL/min as flow rate, 45 °C column temperature and UV detector at 215 nm. The azadirachtin peaks are well resolved and free of interference from matrix components. The extraction and analytical method developed in this work allows the quantitation of azadirachtin with precision and accuracy, establishing a lower limit of quantitation of azadirachtin, extracted from the biological matrix.
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Piergiovanni, Maurizio; Cappiello, Achille; Famiglini, Giorgio; Termopoli, Veronica; Palma, Pierangela
2018-05-30
Dispersive liquid-liquid microextraction with and without ultrasound assistance (DLLME, UA-DLLME) and microextraction with packed sorbent (MEPS) methods for the extraction and determination of eight different benzodiazepines (BDZ) (chlordiazepoxide, flurazepam, bromazepam, oxazepam, lorazepam, clobazam, clonazepam, and flunitrazepam) in three commercial non-alcoholic and light alcoholic beverages were optimized and compared. Benzodiazepines are frequently used for their extensive diffusion and strong numbing effect in drug-facilitated crimes (DFC). The tiny small amount of sample required for DLLME and MEPS extraction makes them very suitable for specimens collected at the crime scene of DFCs. Microextraction techniques are of increasing interest thanks to their accordance to green analytical chemistry (GAC) guidelines providing good recovery values. Ultrasound assistance (UA-DLLME) was used to investigate whether this type of energy can improve the recoveries of the analytes. Analyses of the extracts were performed with reverse-phase capillary high-performance liquid chromatography with UV detection (HPLC - UV), thanks to low environmental impact, robustness, diffusion, and affordability. Recovery percentages at three different concentrations in the three beverages were between 14.30% and 103.28% with intraday and interday RSD lower than ±2.78%. The same samples were extracted using a MEPS protocol, and the results were compared with those obtained with DLLME. MEPS gave recoveries between 20.90% and 101.88% for all matrices showing a better performance than DLLME at higher concentrations, though lower recoveries were observed with diluted samples. Copyright © 2018 Elsevier B.V. All rights reserved.
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Han, Changseok; Likodimos, Vlassis; Khan, Javed Ali; Nadagouda, Mallikarjuna N; Andersen, Joel; Falaras, Polycarpos; Rosales-Lombardi, Pablo; Dionysiou, Dionysios D
2014-10-01
Noble metal Ag-decorated, monodisperse TiO2 aggregates were successfully synthesized by an ionic strength-assisted, simple sol-gel method and were used for the photocatalytic degradation of the antibiotic oxytetracycline (OTC) under both UV and visible light (UV-visible light) irradiation. The synthesized samples were characterized by X-ray diffraction analysis (XRD); UV-vis diffuse reflectance spectroscopy; environmental scanning electron microscopy (ESEM); transmission electron microscopy (TEM); high-resolution TEM (HR-TEM); micro-Raman, energy-dispersive X-ray spectroscopy (EDS); and inductively coupled plasma optical emission spectrometry (ICP-OES). The results showed that the uniformity of TiO2 aggregates was finely tuned by the sol-gel method, and Ag was well decorated on the monodisperse TiO2 aggregates. The absorption of the samples in the visible light region increased with increasing Ag loading that was proportional to the amount of Ag precursor added in the solution over the tested concentration range. The Brunauer, Emmett, and Teller (The BET) surface area slightly decreased with increasing Ag loading on the TiO2 aggregates. Ag-decorated TiO2 samples demonstrated enhanced photocatalytic activity for the degradation of OTC under UV-visible light illumination compared to that of pure TiO2. The sample containing 1.9 wt% Ag showed the highest photocatalytic activity for the degradation of OTC under both UV-visible light and visible light illumination. During the experiments, the detected Ag leaching for the best TiO2-Ag photocatalyst was much lower than the National Secondary Drinking Water Regulation for Ag limit (0.1 mg L(-1)) issued by the US Environmental Protection Agency.
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Gao, Yanyan; Xu, Jianping; Shi, Shaobo; Dong, Hong; Cheng, Yahui; Wei, Chengtai; Zhang, Xiaosong; Yin, Shougen; Li, Lan
2018-04-04
The self-powered ultraviolet photodetectors (UV PDs) have attracted increasing attention due to their potential applications without consuming any external power. It is important to obtain the high-performance self-powered UV PDs by a simple method for the practical application. Herein, TiO 2 nanorod arrays (NRs) were synthesized by hydrothermal method, which were integrated with p-type NiO nanoflakes to realize a high performance pn heterojunction for the efficient UV photodetection. TiO x thin film can improve the morphological and carrier transport properties of TiO 2 NRs and decrease the surface and defect states, resulting in the enhanced photocurrent of the devices. NiO/TiO 2 nanostructural heterojunctions show excellent rectifying characteristics (rectification ratio of 2.52 × 10 4 and 1.45 × 10 5 for NiO/TiO 2 NRs and NiO/TiO 2 NRs/TiO x , respectively) with a very low reverse saturation current. The PDs based on the heterojunctions exhibit good spectral selectivity, high photoresponsivity, and fast response and recovery speeds without external applied bias under the weak light radiation. The devices demonstrate good stability and repeatability under UV light radiation. The self-powered performance could be attributed to the proper built-in electric field of the heterojunction. TiO 2 NRs and NiO nanoflakes construct the well-aligned energy-band structure. The enhanced responsivity and detectivity for the devices with TiO x thin films is related to the increased interfacial charge separation efficiency, reduced carrier recombination, and relatively good electron transport of TiO 2 NRs.
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Hufziger, Kyle T; Bykov, Sergei V; Asher, Sanford A
2017-02-01
We constructed the first deep ultraviolet (UV) Raman standoff wide-field imaging spectrometer. Our novel deep UV imaging spectrometer utilizes a photonic crystal to select Raman spectral regions for detection. The photonic crystal is composed of highly charged, monodisperse 35.5 ± 2.9 nm silica nanoparticles that self-assemble in solution to produce a face centered cubic crystalline colloidal array that Bragg diffracts a narrow ∼1.0 nm full width at half-maximum (FWHM) UV spectral region. We utilize this photonic crystal to select and image two different spectral regions containing resonance Raman bands of pentaerythritol tetranitrate (PETN) and NH 4 NO 3 (AN). These two deep UV Raman spectral regions diffracted were selected by angle tuning the photonic crystal. We utilized this imaging spectrometer to measure 229 nm excited UV Raman images containing ∼10-1000 µg/cm 2 samples of solid PETN and AN on aluminum surfaces at 2.3 m standoff distances. We estimate detection limits of ∼1 µg/cm 2 for PETN and AN films under these experimental conditions.
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Laser-based standoff detection of surface-bound explosive chemicals
NASA Astrophysics Data System (ADS)
Huestis, David L.; Smith, Gregory P.; Oser, Harald
2010-04-01
Avoiding or minimizing potential damage from improvised explosive devices (IEDs) such as suicide, roadside, or vehicle bombs requires that the explosive device be detected and neutralized outside its effective blast radius. Only a few seconds may be available to both identify the device as hazardous and implement a response. As discussed in a study by the National Research Council, current technology is still far from capable of meeting these objectives. Conventional nitrocarbon explosive chemicals have very low vapor pressures, and any vapors are easily dispersed in air. Many pointdetection approaches rely on collecting trace solid residues from dust particles or surfaces. Practical approaches for standoff detection are yet to be developed. For the past 5 years, SRI International has been working toward development of a novel scheme for standoff detection of explosive chemicals that uses infrared (IR) laser evaporation of surfacebound explosive followed by ultraviolet (UV) laser photofragmentation of the explosive chemical vapor, and then UV laser-induced fluorescence (LIF) of nitric oxide. This method offers the potential of long standoff range (up to 100 m or more), high sensitivity (vaporized solid), simplicity (no spectrometer or library of reference spectra), and selectivity (only nitrocompounds).
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The Rapid Detection of Single Bacterial Cells by Deep UV Micro Raman Spectroscopy.
1992-04-01
Saltzman and C.T. Gregg, Appl. Environ. Microbiol. 44, 1081 (1982). 14. D.’. Mc Greggor, W.K. Grace and G.C. Salzman, in "Rapid Methods and...was used by Dr. Marcus Peter of the Dana -Farber Cancer Institute. During that period he came to our laboratories weekly to study GTP- binding
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Fernández-Suárez, Rocío; Ramírez-Villatoro, Guadalupe; Díaz-Ruiz, Gloria; Eslava, Carlos; Calderón, Montserrat; Navarro-Ocaña, Arturo; Trejo-Márquez, Andrea; Wacher, Carmen
2013-01-01
Since Mexico is the second largest exporter of mangoes, its safety assurance is essential. Research in microbial ecology and knowledge of complex interactions among microbes must be better understood to achieve maximal control of pathogens. Therefore, we investigated the effect of UV-C treatments on bacterial diversity of the Ataulfo mangoes surface using PCR-DGGE analysis of variable region V3 of 16S rRNA genes, and the survival of E. coli, by plate counting. The UV-C irradiation reduced the microbial load on the surface of mangoes immediately after treatment and the structure of bacterial communities was modified during storage. We identified the key members of the bacterial communities on the surface of fruits, predominating Enterobacter genus. Genera as Lactococcus and Pantoea were only detected on the surface of non-treated (control) mangoes. This could indicate that these genera were affected by the UV-C treatment. On the other hand, the treatment did not have a significant effect on survival of E. coli. However, genera that have been recognized as antagonists against foodborne pathogens were identified in the bands patterns. Also, phenolic compounds were determined by HPLC and antimicrobial activity was assayed according to the agar diffusion method. The main phenolic compounds were chlorogenic, gallic, and caffeic acids. Mango peel methanol extracts (UV-C treated and control mangoes) showed antimicrobial activity against strains previously isolated from mango, detecting significant differences (P < 0.05) among treated and control mangoes after 4 and 12 days of storage. Ps. fluorescens and Ps. stutszeri were the most sensitive. PMID:23761788
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Neutron detector using sol-gel absorber
Hiller, John M.; Wallace, Steven A.; Dai, Sheng
1999-01-01
An neutron detector composed of fissionable material having ions of lithium, uranium, thorium, plutonium, or neptunium, contained within a glass film fabricated using a sol-gel method combined with a particle detector is disclosed. When the glass film is bombarded with neutrons, the fissionable material emits fission particles and electrons. Prompt emitting activated elements yielding a high energy electron contained within a sol-gel glass film in combination with a particle detector is also disclosed. The emissions resulting from neutron bombardment can then be detected using standard UV and particle detection methods well known in the art, such as microchannel plates, channeltrons, and silicon avalanche photodiodes.
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Results of TLE and TGF Observation in RELEC Experiment onboard "Vernov" Mission
NASA Astrophysics Data System (ADS)
Klimov, Pavel; Garipov, Gali; Klimov, Stanislav; Rothkaehl, Hanna; Khrenov, Boris; Pozanenko, Alexei; Morozenko, Violetta; Iyudin, Anatoly; Bogomolov, Vitalij V.; Svertilov, Sergey; Panasyuk, Mikhail; Saleev, Kirill; Kaznacheeva, Margarita; Maximov, Ivan
2016-07-01
"Vernov" satellite with RELEC experiment onboard was launched on 2014 July, 8 into a polar solar-synchronous orbit. The payload includes DUV ultraviolet and red photometer and DRGE gamma-ray spectrometer providing measurements in 10-3000 keV energy range with four detectors. Both instruments directed to the atmosphere. Total area of DRGE detectors is ˜500 cm ^{2}. The data were recorded both in monitoring and gamma by gamma modes with timing accuracy ˜15 μs. Several TGF candidates with 10-40 gammas in a burst with duration <1 ms were detected. Analysis of data from other instruments on-board "Vernov" satellite shows the absence of significant electromagnetic pulses around correspondent time moments. Comparison with a world wide lightning location network (WWLLN) data base also indicates that there were no thunderstorms connected with most of detected TGF candidates. Possible connection of TGF candidates with electron precipitations is discussed. Observations of transient luminous events (TLEs) were made in UV (240-400 nm) and IR (>610 nm) wavelength bands. More than 8 thousands of flashes with duration between 1 and 128 ms were detected from the atmosphere. Time profiles of detected flashes are very diverse. There are single peak events with significant UV and IR signal, multi-peak structures visible in the both UV and IR channels and very complicated events mixed from UV and IR signals and UV flashes which can continue even during the whole waveform. In addition, there are flashes of various temporal duration and structure measured only in UV wavelength range. Number of UV photons released in the atmosphere varies in a wide range from 10 ^{20} to 10 ^{26}. Apart from the events detected in the thunderstorm regions over the continents, many flashes were observed outside of thunderstorm areas, above the ocean and even at rather high latitudes. Such events are not associated with the thunderstorm and lightning activity measured by WWLLN. Various types of UV and IR flashes measurements and their interpretation, geographical, energy and spectral distribution are presented and discussed.
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Prospects for Near Ultraviolet Astronomical Observations from the Lunar Surface — LUCI
NASA Astrophysics Data System (ADS)
Mathew, J.; Kumar, B.; Sarpotdar, M.; Suresh, A.; Nirmal, K.; Sreejith, A. G.; Safonova, M.; Murthy, J.; Brosch, N.
2018-04-01
We have explored the prospects for UV observations from the lunar surface and developed a UV telescope (LUCI-Lunar Ultraviolet Cosmic Imager) to put on the Moon, with the aim to detect bright UV transients such as SNe, novae, TDE, etc.
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Genetically modified plants for tactical systems applications
NASA Astrophysics Data System (ADS)
Stewart, C. Neal, Jr.
2002-08-01
Plants are ubiquitous in the environment and have the ability to respond to their environment physiologically and through altered gene expression profiles (they cannot walk away). In addition, plant genetic transformation techniques and genomic information in plants are becoming increasingly advanced. We have been performing research to express the jellyfish green fluorescent protein (GFP) in plants. GFP emits green light when excited by blue or UV light. In addition, my group and collaborators have developed methods to detect GFP in plants by contact instruments and at a standoff. There are several tactical uses for this technology. Some obvious applications are using plants as sentinels for detecting biological and chemical warfare agents or their derivatives from a remote platform, as well as detecting explosives. Another tactical application is covert monitoring using individual plants. Different methods to detect GFP in transgenic plants will be discussed.
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Kurt, Hasan; Yüce, Meral; Hussain, Babar; Budak, Hikmet
2016-07-15
In this report, a dual-excitation sensing method was developed using aptamer-functionalized quantum dots and upconverting nanoparticles, exhibiting Stokes and anti-Stokes type excitation profiles, respectively. Conjugation of the aptamer-functionalized luminescent nanoparticles with the magnetic beads, comprising short DNA sequences that were partially complementary to the aptamer sequences, enabled facile separation of the analyte-free conjugates for fluorescent measurement. UV-Visible spectroscopy, Circular Dichroism spectroscopy, Dynamic Light Scattering and Polyacrylamide Gel Electrophoresis techniques were used to characterize the aptamer probes developed. The target-specific luminescent conjugates were applied for multiplex detection of model food pathogens, Salmonella typhimurium, and Staphylococcus aureus, in which the fluorescent emission spectra were obtained under UV excitation at 325nm for quantum dots and NIR excitation at 980nm for upconverting nanoparticles, respectively. The dual-excitation strategy was aimed to minimize cross-talk between the luminescent signals for multiplexed detection, and yielded limit of detection values of 16 and 28cfumL(-1) for Staphylococcus aureus, and Salmonella typhimurium, respectively. By employing a greater number of quantum dots and upconverting nanoparticles with non-overlapping fluorescent emissions, the proposed methodology might be exploited further to detect several analytes, simultaneously. Copyright © 2016 Elsevier B.V. All rights reserved.
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Baltussen, E; Snijders, H; Janssen, H G; Sandra, P; Cramers, C A
1998-04-10
A recently developed method for the extraction of organic micropollutants from aqueous samples based on sorptive enrichment in columns packed with 100% polydimethylsiloxane (PDMS) particles was coupled on-line with HPLC analysis. The sorptive enrichment procedure originally developed for relatively nonpolar analytes was used to preconcentrate polar phenylurea herbicides from aqueous samples. PDMS extraction columns of 5, 10 and 25 cm were used to extract the herbicides from distilled, tap and river water samples. A model that allows prediction of retention and breakthrough volumes is presented. Despite the essentially apolar nature of the PDMS material, it is possible to concentrate sample volumes up to 10 ml on PDMS cartridges without losses of the most polar analyte under investigation, fenuron. For less polar analytes significantly larger sample volumes can be applied. Since standard UV detection does not provide adequate selectivity for river water samples, an electrospray (ES)-MS instrument was used to determine phenylurea herbicides in a water sample from the river Dommel. Methoxuron was present at a level of 80 ng/l. The detection limit of the current set-up, using 10 ml water samples and ES-MS detection is 10 ng/l in river water samples. Strategies for further improvement of the detection limits are identified.
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Sgambelluri, R. Michael; Epis, Sara; Sassera, Davide; Luo, Hong; Angelos, Evan R.; Walton, Jonathan D.
2014-01-01
Species in the mushroom genus Lepiota can cause fatal mushroom poisonings due to their content of amatoxins such as α-amanitin. Previous studies of the toxin composition of poisonous Lepiota species relied on analytical methods of low sensitivity or resolution. Using liquid chromatography coupled to UV absorbance and mass spectrometry, we analyzed the spectrum of peptide toxins present in six Italian species of Lepiota, including multiple samples of three of them collected in different locations. Field taxonomic identifications were confirmed by sequencing of the internal transcribed spacer (ITS) regions. For comparison, we also analyzed specimens of Amanita phalloides from Italy and California, a specimen of A. virosa from Italy, and a laboratory-grown sample of Galerina marginata. α-Amanitin, β-amanitin, amanin, and amaninamide were detected in all samples of L. brunneoincarnata, and α-amanitin and γ-amanitin were detected in all samples of L. josserandii. Phallotoxins were not detected in either species. No amatoxins or phallotoxins were detected in L. clypeolaria, L. cristata, L. echinacea, or L. magnispora. The Italian and California isolates of A. phalloides had similar profiles of amatoxins and phallotoxins, although the California isolate contained more β-amanitin relative to α-amanitin. Amaninamide was detected only in A. virosa. PMID:25098279
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X-ray variability of Seyfert 1.8/1.9 galaxies
NASA Astrophysics Data System (ADS)
Hernández-García, L.; Masegosa, J.; González-Martín, O.; Márquez, I.; Guainazzi, M.; Panessa, F.
2017-06-01
Context. Seyfert 1.8/1.9 are sources showing weak broad Hα components in their optical spectra. According to unification schemes, they are seen with an edge-on inclination, similar to type 2 Seyfert galaxies, but with slightly lower inclination angles. Aims: We aim to test whether Seyfert 1.8/1.9 have similar properties at UV and X-ray wavelengths. Methods: We used the 15 Seyfert 1.8/1.9 in the Véron Cetty and Véron catalog with public data available from the Chandra and/or XMM-Newton archives at different dates, with timescales between observations ranging from days to years. All the spectra of the same source were simultaneously fit with the same model and different parameters were left free to vary in order to select the variable parameter(s). Whenever possible, short-term variations from the analysis of the X-ray light curves and long-term UV variations from the optical monitor onboard XMM-Newton were studied. Our results are homogeneously compared with a previous work using the same methodology applied to a sample of Seyfert 2. Results: X-ray variability is found in all 15 nuclei over the aforementioned ranges of timescales. The main variability pattern is related to intrinsic changes in the sources, which are observed in ten nuclei. Changes in the column density are also frequent, as they are observed in six nuclei, and variations at soft energies, possibly related to scattered nuclear emission, are detected in six sources. X-ray intra-day variations are detected in six out of the eight studied sources. Variations at UV frequencies are detected in seven out of nine sources. Conclusions: A comparison between the samples of Seyfert 1.8/1.9 and 2 shows that, even if the main variability pattern is due to intrinsic changes of the sources in the two families, these nuclei exhibit different variability properties in the UV and X-ray domains. In particular, variations in the broad X-ray band on short timescales (days to weeks), and variations in the soft X-rays and UV on long timescales (months to years) are detected in Seyfert 1.8/1.9 but not in Seyfert 2. Overall, we suggest that optically classified Seyfert 1.8/1.9 should be kept separated from Seyfert 2 galaxies in UV/X-ray studies of the obscured AGN population because their intrinsic properties might be different.
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Trujillo, William A.; Sorenson, Wendy R.; La Luzerne, Paul; Austad, John W.; Sullivan, Darryl
2008-01-01
The presence of aristolochic acid in some dietary supplements is a concern to regulators and consumers. A method has been developed, by initially using a reference method as a guide, during single laboratory validation (SLV) for the determination of aristolochic acid I, also known as aristolochic acid A, in botanical species and dietary supplements at concentrations of approximately 2 to 32 μg/g. Higher levels were determined by dilution to fit the standard curve. Through the SLV, the method was optimized for quantification by liquid Chromatography with ultraviolet detection (LC-UV) and LC/mass Spectrometry (MS) confirmation. The test samples were extracted with organic solvent and water, then injected on a reverse phase LC column. Quantification was achieved with linear regression using a laboratory automation system. The SLV study included systematically optimizing the LC-UV method with regard to test sample size, fine grinding of solids, and solvent extraction efficiency. These parameters were varied in increments (and in separate optimization studies), in order to ensure that each parameter was individually studied; the test results include corresponding tables of parameter variations. In addition, the chromatographic conditions were optimized with respect to injection volume and detection wavelength. Precision studies produced overall relative standard deviation values from 2.44 up to 8.26% for aristolochic acid I. Mean recoveries were between 100 and 103% at the 2 μg/g level, between 102 and 103% at the 10 μg/g level, and 104% at the 30 μg/g level. PMID:16915829
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Trujillo, William A; Sorenson, Wendy R; La Luzerne, Paul; Austad, John W; Sullivan, Darryl
2006-01-01
The presence of aristolochic acid in some dietary supplements is a concern to regulators and consumers. A method has been developed, by initially using a reference method as a guide, during single laboratory validation (SLV) for the determination of aristolochic acid I, also known as aristolochic acid A, in botanical species and dietary supplements at concentrations of approximately 2 to 32 microg/g. Higher levels were determined by dilution to fit the standard curve. Through the SLV, the method was optimized for quantification by liquid chromatography with ultraviolet detection (LC-UV) and LC/mass spectrometry (MS) confirmation. The test samples were extracted with organic solvent and water, then injected on a reverse phase LC column. Quantification was achieved with linear regression using a laboratory automation system. The SLV study included systematically optimizing the LC-UV method with regard to test sample size, fine grinding of solids, and solvent extraction efficiency. These parameters were varied in increments (and in separate optimization studies), in order to ensure that each parameter was individually studied; the test results include corresponding tables of parameter variations. In addition, the chromatographic conditions were optimized with respect to injection volume and detection wavelength. Precision studies produced overall relative standard deviation values from 2.44 up to 8.26% for aristolochic acid I. Mean recoveries were between 100 and 103% at the 2 microg/g level, between 102 and 103% at the 10 microg/g level, and 104% at the 30 microg/g level.
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Granja, Rodrigo H M M; De Lima, Andreia C; Salerno, Alessandro G; Wanschel, Amarylis C B A
2013-01-01
Sulfonamides are one class of antimicrobial agents used in aquaculture production. Sulfonamides are often overused because they are inexpensive and readily available. Their presence at a concentration above the legal limits is a potential hazard to human health. Brazilian authorities have included in the National Regulatory Monitoring Program the control of the three most widely used sulfonamides in aquaculture production, i.e., sulfathiazole, sulfamethazine, and sulfadimethoxine. An LC method with UV detection for the determination of residual sulfonamides in fish muscle, using sulfapyridine as an internal standard has been developed and validated. The validation was performed according to the Brazilian Regulation 24/2009 (equivalent to European Union Decision 2002/657/EC). The method meets the Brazilian regulatory requirement that establishes criteria and procedures for determination of parameters such as decision limit (CCalpha), detection capability (CCbeta), precision, and recovery. For fish muscle, CCalpha was determined at 3.63, 2.91, and 7.46 microg/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. CCbeta was 9.39, 14.54, and 9.39 microg/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. For shrimp, CCalpha was 11.5, 8.67, and 4.46 microg/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. CCbeta was 18, 11.93, and 5.24 microg/kg for sulfathiazole, sulfamethazine, and sulfadimethoxine, respectively. A complete statistical analysis was performed on the results obtained. The results indicate that the method is robust when subjected to day-to-day analytical variations.
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Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo
2017-07-01
Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2 g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.
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Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba; Pirsaheb, Meghdad
2013-11-01
A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma. Copyright © 2013 Elsevier B.V. All rights reserved.
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USDA-ARS?s Scientific Manuscript database
UPLC with UV detection was used for the quantification of alkaloids from roots of Hydrastis canadensis L. (goldenseal) and dietary supplements claiming to contain goldenseal. The chromatographic run time was less than 6 min. The detection wavelengths used were 290 and 344 nm for '-hydrastine, canadi...
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Li, Pingjing; Hu, Bin; Li, Xiaoyong
2012-07-20
In this study, a sensitive, selective and reliable analytical method by combining zirconia (ZrO₂) coated stir bar sorptive extraction (SBSE) with large volume sample stacking capillary electrophoresis-indirect ultraviolet (LVSS-CE/indirect UV) was developed for the direct analysis of chemical warfare agent degradation products of alkyl alkylphosphonic acids (AAPAs) (including ethyl methylphosphonic acid (EMPA) and pinacolyl methylphosphonate (PMPA)) and methylphosphonic acid (MPA) in environmental waters. ZrO₂ coated stir bar was prepared by adhering nanometer-sized ZrO₂ particles onto the surface of stir bar with commercial PDMS sol as adhesion agent. Due to the high affinity of ZrO₂ to the electronegative phosphonate group, ZrO₂ coated stir bars could selectively extract the strongly polar AAPAs and MPA. After systematically optimizing the extraction conditions of ZrO₂-SBSE, the analytical performance of ZrO₂-SBSE-CE/indirect UV and ZrO₂-SBSE-LVSS-CE/indirect UV was assessed. The limits of detection (LODs, at a signal-to-noise ratio of 3) obtained by ZrO₂-SBSE-CE/indirect UV were 13.4-15.9 μg/L for PMPA, EMPA and MPA. The relative standard deviations (RSDs, n=7, c=200 μg/L) of the corrected peak area for the target analytes were in the range of 6.4-8.8%. Enhancement factors (EFs) in terms of LODs were found to be from 112- to 145-fold. By combining ZrO₂ coating SBSE with LVSS as a dual preconcentration strategy, the EFs were magnified up to 1583-fold, and the LODs of ZrO₂-SBSE-LVSS-CE/indirect UV were 1.4, 1.2 and 3.1 μg/L for PMPA, EMPA, and MPA, respectively. The RSDs (n=7, c=20 μg/L) were found to be in the range of 9.0-11.8%. The developed ZrO₂-SBSE-LVSS-CE/indirect UV method has been successfully applied to the analysis of PMPA, EMPA, and MPA in different environmental water samples, and the recoveries for the spiked water samples were found to be in the range of 93.8-105.3%. Copyright © 2012 Elsevier B.V. All rights reserved.
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High performance ultraviolet photodetectors based on ZnO nanoflakes/PVK heterojunction
DOE Office of Scientific and Technical Information (OSTI.GOV)
Cai, Yuhua; Xiang, Jinzhong, E-mail: jzhxiang@ynu.edu.cn; Tang, Libin, E-mail: scitang@163.com
2016-08-15
A high performance ultraviolet (UV) photodetector is receiving increasing attention due to its significant applications in fire warning, environmental monitoring, scientific research, astronomical observation, etc. The enhancement in performance of the UV photodetector has been impeded by lacking of a high-efficiency heterojunction in which UV photons can efficiently convert into charges. In this work, the high performance UV photodetectors have been realized by utilizing organic/inorganic heterojunctions based on a ZnO nanoflakes/poly (N-vinylcarbazole) hybrid. A transparent conducting polymer poly(3,4-ethylene-dioxythiophene):poly(styrenesulfonate)-coated quartz substrate is employed as the anode in replacement of the commonly ITO-coated glass in order to harvest shorter UV light. Themore » devices show a lower dark current density, with a high responsivity (R) of 7.27 × 10{sup 3 }A/W and a specific detectivity (D*) of 6.20 × 10{sup 13} cm Hz{sup 1/2}/W{sup −1} at 2 V bias voltage in ambient environment (1.30 mW/cm{sup 2} at λ = 365 nm), resulting in the enhancements in R and D* by 49% and one order of magnitude, respectively. The study sheds light on developing high-performance, large scale-array, flexible UV detectors using the solution processable method.« less
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Formation of iodinated trihalomethanes during UV/chloramination with iodate as the iodine source.
Zhang, Tian-Yang; Lin, Yi-Li; Wang, An-Qi; Tian, Fu-Xiang; Xu, Bin; Xia, Sheng-Ji; Gao, Nai-Yun
2016-07-01
Iodinated trihalomethanes (I-THMs) are a group of emerging disinfection by-products with high toxicity, and iodide (I(-)) as well as iodinated organic compounds are expected to be their iodine sources. Nevertheless, in this study, iodate (IO3(-)) was proven to be a new iodine source of I-THM formation during UV/chloramination. In the iodate-containing waters (without any other iodine sources), I-THM formation increased with the increase of UV dose, IO3(-) and NH2Cl concentrations. With the increase of Br(-)/IO3(-) molar ratio, I-THM formation (especially for the brominated species) increased. Besides, NOM species could affect I-THM formation from IO3(-) during UV/chloramination. Fulvic acid could promote IO3(-) phototransformation to I(-) but humic acid impeded the production of I(-) during UV irradiation. Under realistic drinking water treatment conditions (DOC = 5.0 mg-C/L, IO3(-) = 12.7 μg-I/L, UV dose = 50 mJ/cm(2), NH2Cl = 5 mg-Cl2/L), CHCl2I was detected as 0.17 μg/L using solid-phase microextraction method, and the production rate of I-THMs from IO3(-) was about 7% of that from I(-). Copyright © 2016 Elsevier Ltd. All rights reserved.
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NASA Technical Reports Server (NTRS)
Torres, Omar; Bhartia, P. K.; Herman, J. R.; Einaudi, Franco (Technical Monitor)
2000-01-01
The interaction between the strong Rayleigh scattering in the near UV spectral region (330-380 nm) and the processes of aerosol absorption and scattering, produce a clear spectral signal in the upwelling radiance at the top of the atmosphere. This interaction is the basis of the TOMS (Total Ozone Mapping Spectrometer) aerosol retrieval technique that can be used for their characterization and to differentiate non-absorbing sulfates from strongly UV-absorbing aerosols such as mineral dust. For absorbing aerosols, the characterization is in terms of the optical depth and single scattering albedo with assumptions about the aerosol plume height. The results for non-absorbing aerosols are not dependent on plume height. Although iron compounds represent only between 5% to 8% of desert dust aerosol mass, hematite (Fe2O3) accounts for most of the near UV absorption. Because of the large ultraviolet absorption characteristic of hematite, the near UV method of aerosol sensing is especially suited for the detection and characterization of desert dust aerosols. Using the combined record of near UV measurements by the Nimbus7 (1978-1992) and Earth Probe (1996-present) TOMS instruments, a global longterm climatology of near UV optical depth and single scattering albedo has been produced. The multi-year long record of mineral aerosol properties over the area of influence of the Saharan desert, will be discussed.
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Insights into quasar UV spectra using unsupervised clustering analysis
NASA Astrophysics Data System (ADS)
Tammour, A.; Gallagher, S. C.; Daley, M.; Richards, G. T.
2016-06-01
Machine learning techniques can provide powerful tools to detect patterns in multidimensional parameter space. We use K-means - a simple yet powerful unsupervised clustering algorithm which picks out structure in unlabelled data - to study a sample of quasar UV spectra from the Quasar Catalog of the 10th Data Release of the Sloan Digital Sky Survey (SDSS-DR10) of Paris et al. Detecting patterns in large data sets helps us gain insights into the physical conditions and processes giving rise to the observed properties of quasars. We use K-means to find clusters in the parameter space of the equivalent width (EW), the blue- and red-half-width at half-maximum (HWHM) of the Mg II 2800 Å line, the C IV 1549 Å line, and the C III] 1908 Å blend in samples of broad absorption line (BAL) and non-BAL quasars at redshift 1.6-2.1. Using this method, we successfully recover correlations well-known in the UV regime such as the anti-correlation between the EW and blueshift of the C IV emission line and the shape of the ionizing spectra energy distribution (SED) probed by the strength of He II and the Si III]/C III] ratio. We find this to be particularly evident when the properties of C III] are used to find the clusters, while those of Mg II proved to be less strongly correlated with the properties of the other lines in the spectra such as the width of C IV or the Si III]/C III] ratio. We conclude that unsupervised clustering methods (such as K-means) are powerful methods for finding `natural' binning boundaries in multidimensional data sets and discuss caveats and future work.
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Electrodialytic in-line preconcentration for ionic solute analysis.
Ohira, Shin-Ichi; Yamasaki, Takayuki; Koda, Takumi; Kodama, Yuko; Toda, Kei
2018-04-01
Preconcentration is an effective way to improve analytical sensitivity. Many types of methods are used for enrichment of ionic solute analytes. However, current methods are batchwise and include procedures such as trapping and elution. In this manuscript, we propose in-line electrodialytic enrichment of ionic solutes. The method can enrich ionic solutes within seconds by quantitative transfer of analytes from the sample solution to the acceptor solution under an electric field. Because of quantitative ion transfer, the enrichment factor (the ratio of the concentration in the sample and to that in the obtained acceptor solution) only depends on the flow rate ratio of the sample solution to the acceptor solution. The ratios of the concentrations and flow rates are equal for ratios up to 70, 20, and 70 for the tested ionic solutes of inorganic cations, inorganic anions, and heavy metal ions, respectively. The sensitivity of ionic solute determinations is also improved based on the enrichment factor. The method can also simultaneously achieve matrix isolation and enrichment. The method was successively applied to determine the concentrations of trace amounts of chloroacetic acids in tap water. The regulated concentration levels cannot be determined by conventional high-performance liquid chromatography with ultraviolet detection (HPLC-UV) without enrichment. However, enrichment with the present method is effective for determination of tap water quality by improving the limits of detection of HPLC-UV. The standard addition test with real tap water samples shows good recoveries (94.9-109.6%). Copyright © 2017 Elsevier B.V. All rights reserved.
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HPLC Determination of Esculin and Esculetin in Rat Plasma for Pharmacokinetic Studies.
Rehman, Shaheed Ur; Kim, In Sook; Kang, Ki Sung; Yoo, Hye Hyun
2015-09-01
An optimized, sensitive and validated reversed-phase high-performance liquid chromatography (RP-HPLC) method with UV detection is described for simultaneous determination of esculin and its aglycone, esculetin, in rat plasma. After addition of internal standard (chrysin), plasma samples were pretreated by solid-phase extraction and introduced into the HPLC system. Analytes were separated on a RP C18 column with a mobile phase of 0.075% acetic acid in water (solvent A) and 90% acetonitrile in solvent A (solvent B) using gradient elution at a flow rate of 1.0 mL/min. The wavelength for UV detection was set at 338 nm. Calibration curves for esculin and esculetin were constructed over a range of 10-1,000 ng/mL. The developed method was found to be specific, precise and accurate. The method was successfully applied to study the pharmacokinetics of esculin and esculetin in rats. After oral administration of 120 mg/kg, the mean Cmax values were 340.3 and 316.5 ng/mL and the AUClast values were 377.3 and 1276.5 h ng/mL for esculin and esculetin, respectively. The bioavailability of esculin was calculated to be 0.62%. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
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Yaripour, Saeid; Mohammadi, Ali; Esfanjani, Isa; Walker, Roderick B; Nojavan, Saeed
2018-01-01
In this study, for the first time, an electro-driven microextraction method named electromembrane extraction combined with a simple high performance liquid chromatography and ultraviolet detection was developed and validated for the quantitation of zolpidem in biological samples. Parameters influencing electromembrane extraction were evaluated and optimized. The membrane consisted of 2-ethylhexanol immobilized in the pores of a hollow fiber. As a driving force, a 150 V electric field was applied to facilitate the analyte migration from the sample matrix to an acceptor solution through a supported liquid membrane. The pHs of donor and acceptor solutions were optimized to 6.0 and 2.0, respectively. The enrichment factor was obtained >75 within 15 minutes. The effect of carbon nanotubes (as solid nano-sorbents) on the membrane performance and EME efficiency was evaluated. The method was linear over the range of 10-1000 ng/mL for zolpidem (R 2 >0.9991) with repeatability ( %RSD) between 0.3 % and 7.3 % ( n = 3). The limits of detection and quantitation were 3 and 10 ng/mL, respectively. The sensitivity of HPLC-UV for the determination of zolpidem was enhanced by electromembrane extraction. Finally, the method was employed for the quantitation of zolpidem in biological samples with relative recoveries in the range of 60-79 %.
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Yaripour, Saeid; Mohammadi, Ali; Esfanjani, Isa; Walker, Roderick B.; Nojavan, Saeed
2018-01-01
In this study, for the first time, an electro-driven microextraction method named electromembrane extraction combined with a simple high performance liquid chromatography and ultraviolet detection was developed and validated for the quantitation of zolpidem in biological samples. Parameters influencing electromembrane extraction were evaluated and optimized. The membrane consisted of 2-ethylhexanol immobilized in the pores of a hollow fiber. As a driving force, a 150 V electric field was applied to facilitate the analyte migration from the sample matrix to an acceptor solution through a supported liquid membrane. The pHs of donor and acceptor solutions were optimized to 6.0 and 2.0, respectively. The enrichment factor was obtained >75 within 15 minutes. The effect of carbon nanotubes (as solid nano-sorbents) on the membrane performance and EME efficiency was evaluated. The method was linear over the range of 10-1000 ng/mL for zolpidem (R2 >0.9991) with repeatability ( %RSD) between 0.3 % and 7.3 % (n = 3). The limits of detection and quantitation were 3 and 10 ng/mL, respectively. The sensitivity of HPLC-UV for the determination of zolpidem was enhanced by electromembrane extraction. Finally, the method was employed for the quantitation of zolpidem in biological samples with relative recoveries in the range of 60-79 %. PMID:29805344
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Wüstner, Daniel; Landt Larsen, Ane; Faergeman, Nils J; Brewer, Jonathan R; Sage, Daniel
2010-04-01
The nematode Caenorhabditis elegans is a genetically tractable model organism to investigate sterol transport. In vivo imaging of the fluorescent sterol, dehydroergosterol (DHE), is challenged by C. elegans' high autofluorescence in the same spectral region as emission of DHE. We present a method to detect DHE selectively, based on its rapid bleaching kinetics compared to cellular autofluorescence. Worms were repeatedly imaged on an ultraviolet-sensitive wide field (UV-WF) microscope, and bleaching kinetics of DHE were fitted on a pixel-basis to mathematical models describing the intensity decay. Bleach-rate constants were determined for DHE in vivo and confirmed in model membranes. Using this method, we could detect enrichment of DHE in specific tissues like the nerve ring, the spermateca and oocytes. We confirm these results in C. elegans gut-granule-loss (glo) mutants with reduced autofluorescence and compare our method with three-photon excitation microscopy of sterol in selected tissues. Bleach-rate-based UV-WF imaging is a useful tool for genetic screening experiments on sterol transport, as exemplified by RNA interference against the rme-2 gene coding for the yolk receptor and for worm homologues of Niemann-Pick C disease proteins. Our approach is generally useful for identifying fluorescent probes in the presence of high cellular autofluorescence.
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Soltaninejad, Kambiz; Karimi, Mohammad; Nateghi, Alireza; Daraei, Bahram
2016-01-01
A high performance liquid chromatographic method with ultra violet detection for simultaneous analysis of six benzodiazepines (BZDs) (chlordiazepoxide, diazepam, clonazepam, midazolam , flurazpam, and lorazepam) has been developed for forensic screening of adulterated non-alcoholic drinks. Samples were analyzed after a simple procedure for preparation using pH adjustment and filtering. Isocratic elution on a C18 column (250mm × 4.6 mm, 5μm) in the temperature 45ºC with a mobile phase consisting of 15mM phosphate buffer: methanol (50:50 v/v) at a flow rate 1.4 mL/min has been done. The column eluent was monitored with a UV detector at 245 nm. This allowed a rapid detection and identification as well as quantization of the eluting peaks. Calibration curves for all drugs in the range of 0.5- 10 µg/ mL that all the linear regression and has more than 0.996. Recovery rates for the BZDs were in the range 93.7- 108.7%. The limits of detection were calculated between 0.01- 0.02 µg/ mL. Also, the limits of quantification were 0.03- 0.05 µg/mL. Within-day and between -day coefficient of variation for all BZDs at all concentrations in the range of 0.45 - 7.69 % was calculated. The procedure can provide a simple, sensitive and fast method for the screening of six BZDs in adulterated soft drinks in forensic analysis. PMID:27642316
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UV-B light contributes directly to the synthesis of chiloglottone floral volatiles
Amarasinghe, Ranamalie; Poldy, Jacqueline; Matsuba, Yuki; Barrow, Russell A.; Hemmi, Jan M.; Pichersky, Eran; Peakall, Rod
2015-01-01
Background and Aims Australian sexually deceptive Chiloglottis orchids attract their specific male wasp pollinators by means of 2,5-dialkylcyclohexane-1,3-diones or ‘chiloglottones’, representing a newly discovered class of volatiles with unique structures. This study investigated the hypothesis that UV-B light at low intensities is directly required for chiloglottone biosynthesis in Chiloglottis trapeziformis. Methods Chiloglottone production occurs only in specific tissue (the callus) of the labellum. Cut buds and flowers, and whole plants with buds and flowers, sourced from the field, were kept in a growth chamber and interactions between growth stage of the flowers and duration and intensity of UV-B exposure on chiloglottone production were studied. The effects of the protein synthesis inhibitor cycloheximide were also examined. Key Results Chiloglottone was not present in buds, but was detected in buds that were manually opened and then exposed to sunlight, or artificial UV-B light for ≥5 min. Spectrophotometry revealed that the sepals and petals blocked UV-B light from reaching the labellum inside the bud. Rates of chiloglottone production increased with developmental stage, increasing exposure time and increasing UV-B irradiance intensity. Cycloheximide did not inhibit the initial production of chiloglottone within 5 min of UV-B exposure. However, inhibition of chiloglottone production by cycloheximide occurred over 2 h of UV-B exposure, indicating a requirement for de novo protein synthesis to sustain chiloglottone production under UV-B. Conclusions The sepals and petals of Chiloglottis orchids strongly block UV-B wavelengths of light, preventing chiloglottone production inside the bud. While initiation of chiloglottone biosynthesis requires only UV-B light, sustained chiloglottone biosynthesis requires both UV-B and de novo protein biosynthesis. The internal amounts of chiloglottone in a flower reflect the interplay between developmental stage, duration and intensity of UV-B exposure, de novo protein synthesis, and feedback loops linked to the starting amount of chiloglottone. It is concluded that UV-B light contributes directly to chiloglottone biosynthesis. These findings suggest an entirely new and unexpected biochemical reaction that might also occur in taxa other than these orchids. PMID:25649114
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NASA Technical Reports Server (NTRS)
Wiebe, D. T.; Zigmond, M. J.; Tufts, C. A.
2002-01-01
The National Aeronautics and Space Administration (NASA) White Sands Test Facility (WSTF) was established in 1963 primarily to provide rocket engine testing services for several NASA programs. The groundwater underlying the site has been contaminated as a result of historical operations. Groundwater contaminants include several volatile organic compounds (VOCs) and two semi-volatile compounds: N-nitrosodimethylamine (NDMA) and N-nitrodimethylamine (DMN). This paper discusses some of the technical, analytical, regulatory, and health risk issues associated with the contaminant plume. The plume has moved approximately 2.5 miles downgradient of the facility industrial boundary, with evidence of continued migration. As a result, NASA has proposed a pump and treat system using air strippers and ultraviolet (UV) oxidation to stabilize future movement of the contaminant plume. The system has been designed to treat 1,076 gallons (4,073 liters) per minute, with provisions for future expansion. The UV oxidation process was selected to treat NDMA-contaminated groundwater based on successes at other NDMA-contaminated sites. Bench- and pilot-scale testing of WSTF groundwater confirmed the ability of UV oxidation to destroy NDMA and generated sufficient data to design the proposed full-scale treatment system. NDMA is acutely toxic and is a probable human carcinogen. EPA-recommended health risk criteria for the residential consumption of NDMA/DMN-contaminated groundwater was used to determine that a 1.0 x 10(exp -6) excess cancer risk corresponds to 1.7 parts per trillion (ppt). EPA analytical methods are unable to detect NDMA and DMN in the low ppt range. EPA's current Appendix IX analytical method used to screen for NDMA, Method 8270, can detect NDMA only at levels that are orders of magnitude greater than the recommended health risk level. Additionally, EPA Method 607, the most sensitive EPA approved method, has a detection limit of 150 ppt. This corresponds to an excess cancer risk of 9.0 x 10(exp -5), which exceeds the State of New Mexico's water quality standard of a cancer risk less than 1 x 10(exp -5). The treatment system has been engineered to treat contaminated groundwater to levels significantly below the New Mexico standard. However, the inability of EPA-approved analytical methods to detect NDMA and DMN at low ppt levels, and to provide verification of compliance with the 1 x 10(exp -5) cancer risk, introduces a notable risk to the long-term operation of the system. WSTF has been working with Southwest Research Institute to develop a non-EPA analytical method that can achieve a reporting limit of 1 ppt, which corresponds to an excess cancer risk of 7.6 x 10(exp -7). WSTF is currently developing a proposal to obtain approval from the New Mexico Environment Department (NMED) of this non-EPA method.
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Liu, Cailing; Vojnovic, Dijana; Kochevar, Irene E.; Jurkunas, Ula V.
2016-01-01
Purpose To examine whether Nrf2-regulated antioxidant defense and p53 are activated in human corneal endothelial cells (CEnCs) by environmental levels of ultraviolet A (UV-A), a known stimulator of oxidative stress. Methods Immortalized human CEnCs (HCEnCi) were exposed to UV-A fluences of 2.5, 5, 10, or 25 J/cm2, then allowed to recover for 3 to 24 hours. Control HCEnCi did not receive UV-A. Reactive oxygen species (ROS) were measured using H2DCFDA. Cell cytotoxicity was evaluated by lactate dehydrogenase (LDH) release. Levels of Nrf2, HO-1, NQO-1, p53, and caspase3 were detected by immunnoblotting or real-time PCR. Activated caspase3 was measured by immunoblotting and a fluorescence assay. Results Exposure of HCEnCi to 5, 10, and 25 J/cm2 UV-A increased ROS levels compared with controls. Nrf2, HO-1, and NQO-1 mRNA increased 1.7- to 3.2-fold at 3 and 6 hours after irradiation with 2.5 and 5 J/cm2 UV-A. At 6 hours post irradiation, UV-A (5 J/cm2) enhanced nuclear Nrf2 translocation. At 24 hours post treatment, UV-A (5, 10, and 25 J/cm2) produced a 1.8- to 2.8-fold increase in phospho-p53 and a 2.6- to 6.0-fold increase in activated caspase3 compared with controls, resulting in 20% to 42% cell death. Conclusions Lower fluences of UV-A induce Nrf2-regulated antioxidant defense and higher fluences activate p53 and caspase3, indicating that even near-environmental levels of UV-A may affect normal CEnCs. This data suggest that UV-A may especially damage cells deficient in antioxidant defense, and thus may be involved in the etiology of Fuchs' endothelial corneal dystrophy (FECD). PMID:27127932
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Werner, S.L.; Johnson, S.M.
1994-01-01
As part of its primary responsibility concerning water as a national resource, the U.S. Geological Survey collects and analyzes samples of ground water and surface water to determine water quality. This report describes the method used since June 1987 to determine selected total-recoverable carbamate pesticides present in water samples. High- performance liquid chromatography is used to separate N-methyl carbamates, N-methyl carbamoyloximes, and an N-phenyl carbamate which have been extracted from water and concentrated in dichloromethane. Analytes, surrogate compounds, and reference compounds are eluted from the analytical column within 25 minutes. Two modes of analyte detection are used: (1) a photodiode-array detector measures and records ultraviolet-absorbance profiles, and (2) a fluorescence detector measures and records fluorescence from an analyte derivative produced when analyte hydrolysis is combined with chemical derivatization. Analytes are identified and confirmed in a three-stage process by use of chromatographic retention time, ultraviolet (UV) spectral comparison, and derivatization/fluorescence detection. Quantitative results are based on the integration of single-wavelength UV-absorbance chromatograms and on comparison with calibration curves derived from external analyte standards that are run with samples as part of an instrumental analytical sequence. Estimated method detection limits vary for each analyte, depending on the sample matrix conditions, and range from 0.5 microgram per liter to as low as 0.01 microgram per liter. Reporting levels for all analytes have been set at 0.5 microgram per liter for this method. Corrections on the basis of percentage recoveries of analytes spiked into distilled water are not applied to values calculated for analyte concentration in samples. These values for analyte concentrations instead indicate the quantities recovered by the method from a particular sample matrix.
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Zhao, Ying-Yong; Zhao, Ye; Zhang, Yong-Min; Lin, Rui-Chao; Sun, Wen-Ji
2009-06-01
Polyporus umbellatus is a widely used anti-aldosteronic diuretic in Traditional Chinese medicine (TCM). A new, sensitive and selective high-performance liquid chromatography-fluorescence detector (HPLC-FLD) and high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS/MS) method for quantitative and qualitative determination of ergosta-4,6,8(14),22-tetraen-3-one(ergone), which is the main diuretic component, was provided for quality control of P. umbellatus crude drug. The ergone in the ethanolic extract of P. umbellatus was unambiguously characterized by HPLC-APCI, and further confirmed by comparing with a standard compound. The trace ergone was detected by the sensitive and selective HPLC-FLD. Linearity (r2 > 0.9998) and recoveries of low, medium and high concentration (100.5%, 100.2% and 100.4%) were consistent with the experimental criteria. The limit of detection (LOD) of ergone was around 0.2 microg/mL. Our results indicated that the content of ergone in P. umbellatus varied significantly from habitat to habitat with contents ranging from 2.13 +/- 0.02 to 59.17 +/- 0.05 microg/g. Comparison among HPLC-FLD and HPLC-UV or HPLC-APCI-MS/MS demonstrated that the HPLC-FLD and HPLC-APCI-MS/MS methods gave similar quantitative results for the selected herb samples, the HPLC-UV methods gave lower quantitative results than HPLC-FLD and HPLC-APCI-MS/MS methods. The established new HPLC-FLD method has the advantages of being rapid, simple, selective and sensitive, and could be used for the routine analysis of P. umbellatus crude drug.
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Zhuang, Shulin; Wang, Haifei; Ding, Keke; Wang, Jiaying; Pan, Liumeng; Lu, Yanli; Liu, Qingjun; Zhang, Chunlong
2016-02-01
Benzotriazole UV stabilizers (BZTs) belong to one prominent group of ultraviolet (UV) stabilizers and are widely used in various plastics materials. Their large production volumes, frequent detections in the environment and potential toxicities have raised increasing public concern. BZTs can be transported in vivo by transport proteins in plasma and the binding association to transport proteins may serve as a significant parameter to evaluate the bioaccumulative potential. We utilized a novel HSA biosensor, circular dichroism spectroscopy, fluorescence spectroscopy to detect the dynamic interactions of six BZTs (UV-326, UV-327, UV-328, UV-329, UV-P, and BZT) with human serum albumin (HSA), and characterized the corresponding structure-activity relationships (SAR) by molecular dynamics simulations. All test BZTs potently bind at Sudlow site I of HSA with a binding constant of 10(4) L/mol at 298 K. Minor changes in the moieties of BZTs affect their interactions with HSA and differently induce conformations of HSA. Their binding reduced electrochemical impedance spectra and α-helix content of HSA, caused slight red-shifted emission, and changed fluorescence lifetime components of HSA in a concentration-dependent mode. UV-327 and UV-329 form hydrogen bonds with HSA, while UV-329, UV-P and BZT bind HSA with more favorable electrostatic interactions. Our in vitro and in silico study offered a significant framework toward the understanding of risk assessment of BZTs and provides guide for future design of environmental benign BZTs-related materials. Copyright © 2015 Elsevier Ltd. All rights reserved.
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NASA Astrophysics Data System (ADS)
Ioannou, Aristos; Daskalakis, Vangelis; Varotsis, Constantinos
2017-08-01
The isolation of reaction products of asparagine with reducing sugars at alkaline pH and high temperature has been probed by a combination of high performance liquid chromatography (HPLC) coupled with a Fraction Collector. The UV-vis and FTIR spectra of the isolated Maillard reaction products showed structure-sensitive changes as depicted by deamination events and formation of asparagine-saccharide conjugates. The initial reaction species of the Asn-Gluc reaction were also characterized by Density Functional Theory (DFT) methods. Evidence for Cu (II) metal ion complexation with the Maillard reaction products is supported by UV-vis and FTIR spectroscopy.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Raso, S.; Ferraro, F. R.; Lanzoni, B.
We used data from the Hubble Space Telescope UV Legacy Survey of Galactic Globular Clusters to select the Blue Straggler Star (BSS) population in four intermediate/high density systems (namely NGC 2808, NGC 6388, NGC 6541, and NGC 7078) through a “UV-guided search.” This procedure consists of using the F275W images in each cluster to construct the master list of detected sources, and then force it to the images acquired in the other filters. Such an approach optimizes the detection of relatively hot stars and allows the detection of a complete sample of BSSs even in the central region of high-densitymore » clusters, because the light from the bright cool giants, which dominates the optical emission in old stellar systems, is sensibly reduced at UV wavelengths. Our UV-guided selections of BSSs have been compared to the samples obtained in previous, optical-driven surveys, clearly demonstrating the efficiency of the UV approach. In each cluster we also measured the parameter A {sup +}, defined as the area enclosed between the cumulative radial distribution of BSSs and that of a reference population, which traces the level of BSS central segregation and the level of dynamical evolution suffered by the system. The values measured for the four clusters studied in this paper nicely fall along the dynamical sequence recently presented for a sample of 25 clusters.« less
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Determination of Prometryne in water and soil by HPLC-UV using cloud-point extraction.
Zhou, Jihai; Chen, Jiandong; Cheng, Yanhong; Li, Daming; Hu, Feng; Li, Huixin
2009-07-15
A CPE-HPLC (UV) method has been developed for the determination of Prometryne. In this method, non-ionic surfactant Triton X-114 was first used to extract and pre-concentrate Prometryne from water and soil samples. The separation and determination of Prometryne were then carried out in an HPLC-UV system with isocratic elution using a detector set at 254 nm wavelength. The parameters and variables that affected the extraction were also investigated and the optimal conditions were found to be 0.5% of Triton X-114 (w/v), 3% of NaCl (w/v) and heat-assisted at 50 degrees C for 30 min. Using these conditions, the recovery rates of Prometryne ranged from 92.84% to 99.23% in water and 85.48% to 93.67% in soil, respectively, with all the relative standard deviations less than 3.05%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.5 microg L(-1) and 11.0 microg L(-1) in water and 4.0 microg kg(-1) and 13.0 microg kg(-1) in soil, respectively. Thus, we developed a method that has proven to be an efficient, green, rapid and inexpensive approach for extraction and determination of Prometryne from soil samples.
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Zhang, Weiqi; Ji, Yinglu; Meng, Jie; Wu, Xiaochun; Xu, Haiyan
2012-01-01
In this work, behaviors of positively-charged AuNRs in a highly metastatic tumor cell line MDA-MB-231 are examined based on UV-vis-NIR absorption spectroscopy in combination with inductively coupled plasma mass spectrometry (ICP-MS), transmission electron microscopy (TEM) and dark-field microscopic observation. It is found that characteristic surface plasmon resonance (SPR) peaks of AuNRs can be detected using spectroscopic method within living cells that have taken up AuNRs. The peak area of transverse SPR band is shown to be proportionally related to the amount of AuNRs in the cells determined with ICP-MS, which suggests a facile and real time quantification method for AuNRs in living cells. The shape of longitudinal SPR band in UV-vis-NIR spectrum reflects the aggregation state of AuNRs in the cells during the incubation period, which is proved by TEM and microscopic observations. Experimental results reveal that AuNRs are internalized by the cells rapidly; the accumulation, distribution and aggregation of AuNRs in the cells compartments are time and dose dependent. The established spectroscopic analysis method can not only monitor the behaviors of AuNRs in living cells but may also be helpful in choosing the optimum laser stimulation wavelength for anti-tumor thermotherapy. PMID:22384113
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UV gated Raman spectroscopy for standoff detection of explosives
NASA Astrophysics Data System (ADS)
Gaft, M.; Nagli, L.
2008-07-01
Real-time detection and identification of explosives at a standoff distance is a major issue in efforts to develop defense against so-called improvised explosive devices (IED). It is recognized that the only method, which is potentially capable to standoff detection of minimal amounts of explosives is laser-based spectroscopy. LDS technique belongs to trace detection, namely to its micro-particles variety. It is based on commonly held belief that surface contamination was very difficult to avoid and could be exploited for standoff detection. We have applied gated Raman spectroscopy for detection of main explosive materials, both factory and homemade. We developed and tested a Raman system for the field remote detection and identification of minimal amounts of explosives on relevant surfaces at a distance of up to 30 m.
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Device and method for determining oxygen concentration and pressure in gases
Ayers, Michael R.; Hunt, Arlon J.
1999-01-01
Disclosed are oxygen concentration and/or pressure sensing devices and methods which incorporate photoluminescent silica aerogels. Disclosed sensors include a light proof housing for holding the photoluminescent aerogel, a source of excitation radiation (e.g., a UV source), a detector for detecting radiation emitted by the aerogel, a system for delivering a sample gas to the aerogel, and a thermocouple. Also disclosed are water resistant oxygen sensors having a photoluminescent aerogel coated with a hydrophobic material.
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Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Zhong, Zhihui
2016-10-01
A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2-500 ng/g, with the correlation coefficients (r) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12-0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25-6.26 % (n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.
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Wang, Yanying; Liu, Yaqin; Ding, Fang; Zhu, Xiaoyan; Yang, Li; Zou, Ping; Rao, Hanbing; Zhao, Qingbiao; Wang, Xianxiang
2018-06-07
In this study, we developed a simple colorimetric approach to detect glutathione (GSH). The proposed approach is based on the ability of CuS-PDA-Au composite material to catalytically oxidize 3,3',5,5'-tetramethylbenzidine (TMB) to ox-TMB to induce a blue color with an absorption peak centered at 652 nm. However, the introduction of GSH can result in a decrease in oxidized TMB; similarly, it can combine with Au nanoparticles (Au NPs) on the surface of CuS-PDA-Au composite material. Both approaches can result in a fading blue color and a reduction of the absorbance at 652 nm. Based on this above, we proposed a technique to detect GSH quantitatively and qualitatively through UV-Vis spectroscopy and naked eye, respectively. This approach demonstrates a low detection limit of 0.42 μM with a broad detection range of 5 × 10 -7 -1 × 10 -4 M with the assistance of UV-Vis spectroscopy. More importantly, this approach is convenient and rapid. This method was successfully applied to GSH detection in human serum and cell lines. Graphical abstract A colorimetric approach has been developed by exploiting the peroxidase-like activity of CuS-polydopamine-Au composite for sensitive glutathione detection.
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Sharma, Manish; Kothari, Charmy; Sherikar, Omkar; Mehta, Priti
2014-01-01
Accurate, sensitive and reproducible reversed-phase high-performance liquid chromatography (RP-HPLC), high-performance thin-layer chromatography (HPTLC) and ultraviolet (UV) spectrophopometric methods were developed for the concurrent estimation of amlodipine besylate (AMLO), hydrochlorothiazide (HCTZ) and valsartan (VALS) in bulk and combined tablet dosage forms. For the RP-HPLC method, separation was achieved on a C18 column using potassium dihydrogen orthophosphate buffer (50 mM, pH 3.7) with 0.2% triethylamine as the modifier and acetonitrile in the ratio of 56:44 (v/v) as the mobile phase. Quantification was achieved using a photodiode array detector at 232 nm over a concentration range of 2-25 µg/mL for AMLO, 5-45 µg/mL for HCTZ and 20-150 µg/mL for VALS. For the HPTLC method, the drugs were separated by using ethyl acetate-methanol-toluene-ammonia (7.5:3:2:0.8, v/v/v/v) as the mobile phase. Quantification was achieved using UV detection at 242 nm over a concentration range of 100-600 ng/spot for AMLO, 150-900 ng/spot for HCTZ and 1,200-3,200 ng/spot for VALS. The UV-spectrophotometric simultaneous equation method was based on the measurement of absorbance at three wavelengths; i.e., at 237.6 nm (λmax of AMLO), 270.2 nm (λmax of HCTZ) and 249.2 nm (λmax of VALS) in methanol. Quantification was achieved over the concentration range of 2-20 µg/mL for AMLO, 5-25 µg/mL HCTZ and 10-50 µg/mL for VALS. All methods were validated according to International Conference on Harmonization guidelines and successfully applied to marketed pharmaceutical formulations. Additionally, the three methods were compared statistically by an analysis of variance test, which revealed no significant difference between the proposed methods with respect to accuracy and precision.
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Lin, Chung-Ho; Lerch, Robert N.; Thurman, E. Michael; Garrett , Harold E.; George, Milon F.
2002-01-01
Balance (isoxaflutole, IXF) belongs to a new family of herbicides referred to as isoxazoles. IXF has a very short soil half-life (<24 h), degrading to a biologically active diketonitrile (DKN) metabolite that is more polar and considerably more stable. Further degradation of the DKN metabolite produces a nonbiologically active benzoic acid (BA) metabolite. Analytical methods using solid phase extraction followed by high-performance liquid chromatography−UV (HPLC-UV) or high-performance liquid chromatography−mass spectrometry (HPLC-MS) were developed for the analysis of IXF and its metabolites in distilled deionized water and ground water samples. To successfully detect and quantify the BA metabolite by HPLC-UV from ground water samples, a sequential elution scheme was necessary. Using HPLC-UV, the mean recoveries from sequential elution of the parent and its two metabolites from fortified ground water samples ranged from 68.6 to 101.4%. For HPLC-MS, solid phase extraction of ground water samples was performed using a polystyrene divinylbenzene polymer resin. The mean HPLC-MS recoveries of the three compounds from ground water samples spiked at 0.05−2 μg/L ranged from 100.9 to 110.3%. The limits of quantitation for HPLC-UV are approximately 150 ng/L for IXF, 100 ng/L for DKN, and 250 ng/L for BA. The limit of quantitation by HPLC-MS is 50 ng/L for each compound. The methods developed in this work can be applied to determine the transport and fate of Balance in the environment.
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Lin, Chung-Ho; Lerch, Robert N; Thurman, E Michael; Garrett, Harold E; George, Milon F
2002-10-09
Balance (isoxaflutole, IXF) belongs to a new family of herbicides referred to as isoxazoles. IXF has a very short soil half-life (<24 h), degrading to a biologically active diketonitrile (DKN) metabolite that is more polar and considerably more stable. Further degradation of the DKN metabolite produces a nonbiologically active benzoic acid (BA) metabolite. Analytical methods using solid phase extraction followed by high-performance liquid chromatography-UV (HPLC-UV) or high-performance liquid chromatography-mass spectrometry (HPLC-MS) were developed for the analysis of IXF and its metabolites in distilled deionized water and ground water samples. To successfully detect and quantify the BA metabolite by HPLC-UV from ground water samples, a sequential elution scheme was necessary. Using HPLC-UV, the mean recoveries from sequential elution of the parent and its two metabolites from fortified ground water samples ranged from 68.6 to 101.4%. For HPLC-MS, solid phase extraction of ground water samples was performed using a polystyrene divinylbenzene polymer resin. The mean HPLC-MS recoveries of the three compounds from ground water samples spiked at 0.05-2 microg/L ranged from 100.9 to 110.3%. The limits of quantitation for HPLC-UV are approximately 150 ng/L for IXF, 100 ng/L for DKN, and 250 ng/L for BA. The limit of quantitation by HPLC-MS is 50 ng/L for each compound. The methods developed in this work can be applied to determine the transport and fate of Balance in the environment.
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NASA Astrophysics Data System (ADS)
Hashimoto, M.; Kuze, A.; Bruegge, C. J.; Shiomi, K.; Kataoka, F.; Kikuchi, N.; Arai, T.; Kasai, K.; Nakajima, T.
2016-12-01
The GOSAT (Greenhouse Gases Observing Satellite) / TANSO-CAI (Cloud and Aerosol Imager, CAI) is an imaging sensor to measure cloud and aerosol properties and observes reflected sunlight from the atmosphere and surface of the ground. The sensor has four bands from near ultraviolet (near-UV) to shortwave infrared, 380, 674, 870 and 1600nm. The field of view size is 0.5 km for band-1 through band-3, and 1.5km for band-4. Band-1 (380nm) is one of unique function of the CAI. The near-UV observation offers several advantages for the remote sensing of aerosols over land: Low reflectance of most surfaces; Sensitivity to absorbing aerosols; Absorption of trace gases is weak (Höller et al., 2004). CAI UV-band is useful to distinguish absorbing aerosol (smoke) from cloud. GOSAT-2/TANSO-CAI-2 that will be launched in the future also has UV-bands, 340 and 380nm. We carried out an experiment to calibrate CAI UV-band radiance using data taken in a field campaign of OCO-2 and GOSAT at Railroad Valley in 2016. The campaign period is June 27 to July 3 in 2016. We measured surface reflectance by using USB4000 Spectrometer with 74-UV collimating lens (Ocean Optics) and Spectralon (Labsphere). USB4000 is a UV spectrometer, and its measurement range from 300 to 520nm. We simulated CAI UV-band radiance using a vector type of radiation transfer code, i.e. including polarization calculation, pstar3 (Ota et al., 2010) using measured surface reflectance and atmospheric data, pressure and relative humidity by radiosonde in the same campaign, and aerosol optical depth by AERONET, etc. Then, we evaluated measured UV radiances with the simulated data. We show the result of vicarious calibration of CAI UV-band in the campaign, and discuss about this method for future sensor, CAI-2. Around the campaign period, there was wildfire around Los Angeles, and aerosol optical thickness (AOT) observed by AERONET at Rail Road valley and Caltech sites is also high. We tried to detect and retrieve aerosol properties using CAI data around campaign region by the multi-wavelength and multi-pixel method (MWPM) (Hashimoto AGU Fall meeting, 2014) using CAI UV-band. In the analysis, we use CAI four bands to retrieve aerosol optical properties including cloud optical characteristics. We also like to introduce the analysis result of aerosol optical properties during wildfire.
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Lorenz, Dominic; Erasmy, Nicole; Akil, Youssef; Saake, Bodo
2016-04-20
A new method for the chemical characterization of xylans is presented, to overcome the difficulties in quantification of 4-O-methyl-α-D-glucuronic acid (meGlcA). In this regard, the hydrolysis behavior of xylans from beech and birch wood was investigated to obtain the optimum conditions for hydrolysis, using sulfuric acid. Due to varying linkage strengths and degradation, no general method for complete hydrolysis can be designed. Therefore, partial hydrolysis was applied, yielding monosaccharides and small meGlcA containing oligosaccharides. For a new method by HPAEC-UV/VIS, these samples were reductively aminated by 2-aminobenzoic acid. By quantification of monosaccharides and oligosaccharides, as well as comparison with borate-HPAEC and (13)C NMR-spectroscopy, we revealed that the concentrations meGlcA are significantly underestimated compared to conventional methods. The detected concentrations are 85.4% (beech) and 76.3% (birch) higher with the new procedure. Furthermore, the quantified concentrations of xylose were 9.3% (beech) and 6.5% (birch) higher by considering the unhydrolyzed oligosaccharides as well. Copyright © 2015 Elsevier Ltd. All rights reserved.
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Musmade, Kranti P.; Trilok, M.; Dengale, Swapnil J.; Bhat, Krishnamurthy; Reddy, M. S.; Musmade, Prashant B.; Udupa, N.
2014-01-01
A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC) method with UV detection has been developed and validated for quantification of naringin (NAR) in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by employing a C18 (250.0 × 4.6 mm, 5 μm) column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v) as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1). The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV) less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity. PMID:26556205
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A UV-Vis photoacoustic spectrophotometer.
Wiegand, Joseph R; Mathews, L Dalila; Smith, Geoffrey D
2014-06-17
A novel photoacoustic spectrophotometer (PAS) for the measurement of gas-phase and aerosol absorption over the UV-visible region of the spectrum is described. Light from a broadband Hg arc lamp is filtered in eight separate bands from 300 to 700 nm using bandpass interference filters (centered at 301 nm, 314 nm, 364 nm, 405 nm, 436 nm, 546 nm, 578 and 687 nm) and modulated with an optical chopper before entering the photoacoustic cell. All wavelength bands feature a 20-s detection limit of better than 3.0 Mm(-1) with the exception of the lower-intensity 687 nm band for which it is 10.2 Mm(-1). Validation measurements of gas-phase acetone and nigrosin aerosol absorption cross sections at several wavelengths demonstrate agreement to within 10% with those measured previously (for acetone) and those predicted by Mie theory (for nigrosin). The PAS instrument is used to measure the UV-visible absorption spectrum of ambient aerosol demonstrating a dramatic increase in the UV region with absorption increasing by 300% from 405 to 301 nm. This type of measurement throughout the UV-visible region and free from artifacts associated with filter-based methods has not been possible previously, and we demonstrate its promise for classifying and quantifying different types of light-absorbing ambient particles.
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Van Beek, T A; Blaakmeer, A
1989-03-03
A method has been developed for the quantitation of the bitter component limonin in grapefruit juice and other citrus juices. The sample clean-up consisted of centrifugation, filtration and a selective, rapid and reproducible purification with a C2 solid-phase extraction column. The limonin concentration was determined by high-performance liquid chromatography on a C18 column with UV detection at 210 nm. A linear response was obtained from 0.0 to 45 ppm limonin. The minimum detectable amount was 2 ng. The minimum concentration which was detected without concentration with good precision was 0.1 ppm. The method was also used for the determination of limonin in different types of oranges, including navel oranges, mandarins, lemons, limes, pomelos and uglis.
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Isolation of uv-sensitive variants of human FL cells by a viral suicide method
DOE Office of Scientific and Technical Information (OSTI.GOV)
Shiomi, T.; Sato, K.
A new method (viral suicide method) for the isolation of uv-sensitive mutants is described. Colonies of mutagenized human FL cells were infected with uv-irradiated Herpes simplex viruses and surviving ones which seemed to be deficient in host cell reactivation (HCR) were examined for their uv sensitivity. Nineteen of 238 clones examined were sensitive to uv irradiation at the time of the isolation. After recloning, four of these clones have been studied and two (UVS-1 and UVS-2) of them are stable in their uv sensitivity for 4 months in culture. uv sensitivity of UVS-1, UVS-2, and the parental FL cells aremore » as follows: the extrapolation numbers (n) are 2.2, 2.1, and 1.8 and mean lethal doses (DO) are 2.9, 3.7, and 7.8 J/m/sup 2/ for UVS-1, UVS-2, and the parental FL cells, respectively. They are no more sensitive than FL cells to x-irradiation. The ability of HCR in UVS-2 cells is apparently lower than that in FL cells, whereas UVS-1 cells are the same as FL cells in the ability.« less
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Hu, Yang; Zhang, Jing; Lv, Yuan-Zheng; Huang, Xiao-Huan; Hu, Sheng-Li
2016-03-15
A new colorimetric probe 1 based on rhodamine B lactam was developed for naked-eye detection of Cu(2+). The optical feature of 1 for Cu(2+) was investigated by UV-vis absorption spectroscopy. Upon the addition of Cu(2+), the 1 displayed a distinct color change from colorless to pink, which can be directly detected by the naked eye. The stoichiometry of 1 to Cu(2+) complex was found to be 1:1 and the naked-eye detection limit was determined as low as 2 μM. The results suggest that the probe 1 may provide a convenient method for visual detection of Cu(2+) with high sensitivity. Copyright © 2015 Elsevier B.V. All rights reserved.
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Hao, Guitang; Chen, Shangwei; Zhu, Song; Yin, Hongping; Dai, Jun; Cao, Yuhua
2007-01-01
An ion-pair reversed-phase high performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of carbohydrate and uronic acids was developed. p-Aminobenzoic acid (p-AMBA) was used for pre-column derivatization of the analytes, enabling fluorescence (lambda(ex) = 313 nm, lambda(em) = 358 nm) or ultraviolet (UV at 303 nm) detection. Reaction conditions such as reaction temperature and reaction time were optimized. Atlantis dC18 column with hydrophilic end capping was selected for the separation of derivatives. Effects of mobile phase compositions such as ion pairs and their concentrations and pH on the retention behaviors and separation results of 9 monosaccharides and 2 uronic acids were investigated. Derivatives of fructose, galactose, glucose, mannose, xylose, arabinose, ribose, galacturonic acid, fucose, glucuronic acid and rhamnose were separated within 42 min, applying tetrabutyl ammonium hydrogen bisulfate (TBAHSO4) as the ion pair reagent. The detection limits were between 3.38 x 10(-8) mol/L and 176 x 10(-8) mol/L for fluorescence detection and between 2.55 x 10(-7) mol/L and 13.4 x 10(-7) mol/L for UV detection. Good linearities were obtained with correlation coefficients (r2) above 0.99. The relative standard deviations (RSDs) of the peak area of the derivatives in 12 - 51 h after derivatization were from 2.5% to 3.9%. This method has been applied for the determination of mono-/disaccharides and uronic acids in spirulina polysaccharide after dissolved in trifluoroacetic acid solution (2 mol/L). The results showed this method is suitable for the analysis of monosaccharide compositions in polysaccharides.
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Code of Federal Regulations, 2013 CFR
2013-10-01
... samples are analyzed directly by high performance liquid chromatography (HPLC). Detection limits: 0.01% by... proper selection of HPLC parameters. 2.4. Samples must be free of any particulates that may clog the... clarification kit. 3. Apparatus 3.1. Liquid chromatograph equipped with a UV detector. 3.2. HPLC Column that...
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Code of Federal Regulations, 2012 CFR
2012-10-01
... samples are analyzed directly by high performance liquid chromatography (HPLC). Detection limits: 0.01% by... proper selection of HPLC parameters. 2.4. Samples must be free of any particulates that may clog the... clarification kit. 3. Apparatus 3.1. Liquid chromatograph equipped with a UV detector. 3.2. HPLC Column that...
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Code of Federal Regulations, 2014 CFR
2014-10-01
... samples are analyzed directly by high performance liquid chromatography (HPLC). Detection limits: 0.01% by... proper selection of HPLC parameters. 2.4. Samples must be free of any particulates that may clog the... clarification kit. 3. Apparatus 3.1. Liquid chromatograph equipped with a UV detector. 3.2. HPLC Column that...
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Evidence for instantaneous e-vector detection in the honeybee using an associative learning paradigm
Sakura, Midori; Okada, Ryuichi; Aonuma, Hitoshi
2012-01-01
Many insects use the polarization pattern of the sky for obtaining compass information during orientation or navigation. E-vector information is collected by a specialized area in the dorsal-most part of the compound eye, the dorsal rim area (DRA). We tested honeybees' capability of learning certain e-vector orientations by using a classical conditioning paradigm with the proboscis extension reflex. When one e-vector orientation (CS+) was associated with sugar water, while another orientation (CS−) was not rewarded, the honeybees could discriminate CS+ from CS−. Bees whose DRA was inactivated by painting did not learn CS+. When ultraviolet (UV) polarized light (350 nm) was used for CS, the bees discriminated CS+ from CS−, but no discrimination was observed in blue (442 nm) or green light (546 nm). Our data indicate that honeybees can learn and discriminate between different e-vector orientations, sensed by the UV receptors of the DRA, suggesting that bees can determine their flight direction from polarized UV skylight during foraging. Fixing the bees' heads during the experiments did not prevent learning, indicating that they use an ‘instantaneous’ algorithm of e-vector detection; that is, the bees do not need to actively scan the sky with their DRAs (‘sequential’ method) to determine e-vector orientation. PMID:21733901
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Acosta, Gimena; Spisso, Adrián; Fernández, Liliana P; Martinez, Luis D; Pacheco, Pablo H; Gil, Raúl A
2015-03-15
A high performance liquid chromatography coupled with atomic fluorescence spectrometry method for the determination of thimerosal (sodium ethylmercury thiosalicylate, C9H9HgNaO2S), ethylmercury, and inorganic mercury is proposed. Mercury vapor is generated by the post-column reduction of mercury species in formic acid media using UV-radiation. Thimerosal is quantitatively converted to Hg(II) followed by the reduction of Hg(II) to Hg(0). This method is applied to the determination of thimerosal (THM), ethylmercury (EtHg) and inorganic Hg in samples of a pharmaceutical industry effluent, and in waters of the San Luis River situated in the west side of San Luis city (Middle West, Argentine) where the effluents are dumped. The limit of detections, calculated on the basis of the 3σ criterion, where 0.09, 0.09 and 0.07 μg L(-1) for THM, EtHg(II) and for Hg(II), respectively. Linearity was attained from levels close to the detection limit up to at least 100 μg L(-1). Copyright © 2014 Elsevier B.V. All rights reserved.
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Zheng, Yunliang; Luan, Lianjun; Chen, Yong; Ren, Yiping; Wu, Yongjiang
2012-12-01
Physalins are important bioactive compounds from genus Physalis. They often occur as isomers, which makes the structural elucidation difficult. In the present study, the fragmentation behavior and UV characteristics of seven physalins from genus Physalis were firstly investigated using electrospray ionization tandem mass spectrometry (ESI-MS/MS) and diode array detection (DAD). Combined with ultra-performance liquid chromatography (UPLC) and DAD, the established approach to the structural identification of physalins by ESI-MS/MS was then applied to the analysis of Physalis alkekengi L. According to the UPLC retention behavior, the diagnostic UV spectra and the molecular structural information provided by MS/MS spectra, about 19 fingerprint peaks were identified, including 14 physalins and 5 other compounds. Finally, the established fingerprint method was applied to the analysis of 31 P. alkekengi L. samples collected from different locations, which reflected their similar chemical constituent properties. The proposed method provides a scientific and technical platform to the herbal industry for quality control and safety assurance of herbal preparations that contain this class of physalins. Copyright © 2012 Elsevier B.V. All rights reserved.
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Fluorescence properties of human teeth and dental calculus for clinical applications
NASA Astrophysics Data System (ADS)
Lee, Yong-Keun
2015-04-01
Fluorescent emission of human teeth and dental calculus is important for the esthetic rehabilitation of teeth, diagnosis of dental caries, and detection of dental calculus. The purposes of this review were to summarize the fluorescence and phosphorescence of human teeth by ambient ultraviolet (UV) light, to investigate the clinically relevant fluorescence measurement methods in dentistry, and to review the fluorescence of teeth and dental calculus by specific wavelength light. Dentine was three times more phosphorescent than enamel. When exposed to light sources containing UV components, the fluorescence of human teeth gives them the quality of vitality, and fluorescent emission with a peak of 440 nm is observed. Esthetic restorative materials should have fluorescence properties similar to those of natural teeth. Based on the fluorescence of teeth and restorative materials as determined with a spectrophotometer, a fluorescence parameter was defined. As to the fluorescence spectra by a specific wavelength, varied wavelengths were investigated for clinical applications, and several methods for the diagnosis of dental caries and the detection of dental calculus were developed. Since fluorescent properties of dental hard tissues have been used and would be expanded in diverse fields of clinical practice, these properties should be investigated further, embracing newly developed optical techniques.
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Fluorescence properties of human teeth and dental calculus for clinical applications.
Lee, Yong-Keun
2015-04-01
Fluorescent emission of human teeth and dental calculus is important for the esthetic rehabilitation of teeth, diagnosis of dental caries, and detection of dental calculus. The purposes of this review were to summarize the fluorescence and phosphorescence of human teeth by ambient ultraviolet (UV) light, to investigate the clinically relevant fluorescence measurement methods in dentistry, and to review the fluorescence of teeth and dental calculus by specific wavelength light. Dentine was three times more phosphorescent than enamel. When exposed to light sources containing UV components, the fluorescence of human teeth gives them the quality of vitality, and fluorescent emission with a peak of 440 nm is observed. Esthetic restorative materials should have fluorescence properties similar to those of natural teeth. Based on the fluorescence of teeth and restorative materials as determined with a spectrophotometer, a fluorescence parameter was defined. As to the fluorescence spectra by a specific wavelength, varied wavelengths were investigated for clinical applications, and several methods for the diagnosis of dental caries and the detection of dental calculus were developed. Since fluorescent properties of dental hard tissues have been used and would be expanded in diverse fields of clinical practice, these properties should be investigated further, embracing newly developed optical techniques.
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Wang, Xin; Gao, Jun; Fan, Zhiguo
2014-02-01
It is surprising that many insect species use only the ultraviolet (UV) component of the polarized skylight for orientation and navigation purposes, while both the intensity and the degree of polarization of light from the clear sky are lower in the UV than at longer (blue, green, red) wavelengths. Why have these insects chosen the UV part of the polarized skylight? This strange phenomenon is called the "UV-sky-pol paradox". Although earlier several speculations tried to resolve this paradox, they did this without any quantitative data. A theoretical and computational model has convincingly explained why it is advantageous for certain animals to detect celestial polarization in the UV. We performed a sky-polarimetric approach and built a polarized skylight sensor that models the processing of polarization signals by insect photoreceptors. Using this model sensor, we carried out measurements under clear and cloudy sky conditions. Our results showed that light from the cloudy sky has maximal degree of polarization in the UV. Furthermore, under both clear and cloudy skies the angle of polarization of skylight can be detected with a higher accuracy. By this, we corroborated empirically the soundness of the earlier computational resolution of the UV-sky-pol paradox.
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NASA Astrophysics Data System (ADS)
Wang, Xin; Gao, Jun; Fan, Zhiguo
2014-02-01
It is surprising that many insect species use only the ultraviolet (UV) component of the polarized skylight for orientation and navigation purposes, while both the intensity and the degree of polarization of light from the clear sky are lower in the UV than at longer (blue, green, red) wavelengths. Why have these insects chosen the UV part of the polarized skylight? This strange phenomenon is called the "UV-sky-pol paradox". Although earlier several speculations tried to resolve this paradox, they did this without any quantitative data. A theoretical and computational model has convincingly explained why it is advantageous for certain animals to detect celestial polarization in the UV. We performed a sky-polarimetric approach and built a polarized skylight sensor that models the processing of polarization signals by insect photoreceptors. Using this model sensor, we carried out measurements under clear and cloudy sky conditions. Our results showed that light from the cloudy sky has maximal degree of polarization in the UV. Furthermore, under both clear and cloudy skies the angle of polarization of skylight can be detected with a higher accuracy. By this, we corroborated empirically the soundness of the earlier computational resolution of the UV-sky-pol paradox.
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Yu, Jiawen; Xu, Hongjuan; Mo, Zhihong; Zhu, Huali; Mao, Xianbing
2009-07-01
A simple and sensitive reversed-phase liquid chromatographic method, based on the precolumn derivatization with 9-fluorenylmethyl chloroformate, was developed for the determination of myriocin. The derivatization reaction was performed in organic solvents of pyridine and tetrahydrofuran at 40 degrees C. Several factors influencing the derivative yield were investigated and optimized. The formed derivative was stable for more than 24 h at room temperature. The detection wavelength was 262 nm. The system offered the following analytical parameters: the limit of detection was 0.045 microg ml(-1), the linear correlation coefficient was 0.9963 and the linear range response was from 2.0 to 500.0 microg ml(-1). The precision of the method was <2.0%. As a preliminary application, the method has been successfully applied to the determination of myriocin in natural and cultured Cordyceps cicadae.
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Mengerink, Y; Peters, R; Kerkhoff, M; Hellenbrand, J; Omloo, H; Andrien, J; Vestjens, M; van der Wal, S
2000-05-05
By separating the first six linear and cyclic oligomers of polyamide-6 on a reversed-phase high-performance liquid chromatographic system after sandwich injection, quantitative determination of these oligomers becomes feasible. Low-wavelength UV detection of the different oligomers and selective post-column reaction detection of the linear oligomers with o-phthalic dicarboxaldehyde (OPA) and 3-mercaptopropionic acid (3-MPA) are discussed. A general methodology for quantification of oligomers in polymers was developed. It is demonstrated that the empirically determined group-equivalent absorption coefficients and quench factors are a convenient way of quantifying linear and cyclic oligomers of nylon-6. The overall long-term performance of the method was studied by monitoring a reference sample and the calibration factors of the linear and cyclic oligomers.
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NASA Astrophysics Data System (ADS)
Liu, Chuanwu; Mutch, Simon J.; Angel, P. W.; Duffy, Alan R.; Geil, Paul M.; Poole, Gregory B.; Mesinger, Andrei; Wyithe, J. Stuart B.
2016-10-01
In this paper, we present calculations of the UV luminosity function (LF) from the Dark-ages Reionization And Galaxy-formation Observables from Numerical Simulations project, which combines N-body, semi-analytic and seminumerical modelling designed to study galaxy formation during the Epoch of Reionization. Using galaxy formation physics including supernova feedback, the model naturally reproduces the UV LFs for high-redshift star-forming galaxies from z ˜ 5 through to z ˜ 10. We investigate the luminosity-star formation rate (SFR) relation, finding that variable SFR histories of galaxies result in a scatter around the median relation of 0.1-0.3 dex depending on UV luminosity. We find close agreement between the model and observationally derived SFR functions. We use our calculated luminosities to investigate the LF below current detection limits, and the ionizing photon budget for reionization. We predict that the slope of the UV LF remains steep below current detection limits and becomes flat at MUV ≳ -14. We find that 48 (17) per cent of the total UV flux at z ˜ 6 (10) has been detected above an observational limit of MUV ˜ -17, and that galaxies fainter than MUV ˜ -17 are the main source of ionizing photons for reionization. We investigate the luminosity-stellar mass relation, and find a correlation for galaxies with MUV < -14 that has the form M_{ast } ∝ 10^{-0.47M_UV}, in good agreement with observations, but which flattens for fainter galaxies. We determine the luminosity-halo mass relation to be M_vir ∝ 10^{-0.35M_UV}, finding that galaxies with MUV = -20 reside in host dark matter haloes of 1011.0±0.1 M⊙ at z ˜ 6, and that this mass decreases towards high redshift.
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Pretorius, Carel J; McWhinney, Brett C; Sipinkoski, Bilyana; Wilce, Alice; Cox, David; McWhinney, Avis; Ungerer, Jacobus P J
2018-03-01
We optimized a quantitative amino acid method with pre-column derivatization, norvaline (nva) internal standard and reverse phase ultra-performance liquid chromatography by replacing the ultraviolet detector with a single quadrupole mass spectrometer (MS nva ). We used 13 C 15 N isotopically labeled amino acid internal standards and a C18 column with 1.6μm particles to optimize the chromatography and to confirm separation of isobaric compounds (MS lis ). We compared the analytical performance of MS nva with MS lis and the original method (UV nva ) with clinical samples. The chromatography time per sample of MS nva was 8min, detection capabilities were <1μmol/L for most components, intermediate imprecisions at low concentrations were <10% and there was negligible carryover. MS nva was linear up to a total amino acid concentration in a sample of approximately 9500μmol/L. The agreements between most individual amino acids were satisfactory compared to UV nva with the latter prone to outliers and suboptimal quantitation of urinary arginine, aspartate, glutamate and methionine. MS nva reliably detected argnininosuccinate, β-alanine, citrulline and cysteine-s-sulfate. MS nva resulted in a more than fivefold increase in operational efficiency with accurate detection of amino acids and metabolic intermediates in clinical samples. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.
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NASA Astrophysics Data System (ADS)
Cho, Hyunjeong; Baek, Insuck; Oh, Mirae; Kim, Sungyoun; Lee, Hoonsoo; Kim, Moon S.
2017-05-01
Bacterial biofilm formed by pathogens on fresh produce surfaces is a food safety concern because the complex extracellular matrix in the biofilm structure reduces the reduction and removal efficacies of washing and sanitizing processes such as chemical or irradiation treatments. Therefore, a rapid and nondestructive method to identify pathogenic biofilm on produce surfaces is needed to ensure safe consumption of fresh, raw produce. This research aimed to evaluate the feasibility of hyperspectral fluorescence imaging for detecting Escherichia.coli (ATCC 25922) biofilms on baby spinach leaf surfaces. Samples of baby spinach leaves were immersed and inoculated with five different levels (from 2.6x104 to 2.6x108 CFU/mL) of E.coli and stored at 4°C for 24 h and 48 h to induce biofilm formation. Following the two treatment days, individual leaves were gently washed to remove excess liquid inoculums from the leaf surfaces and imaged with a hyperspectral fluorescence imaging system equipped with UV-A (365 nm) and violet (405 nm) excitation sources to evaluate a spectral-image-based method for biofilm detection. The imaging results with the UV-A excitation showed that leaves even at early stages of biofilm formations could be differentiated from the control leaf surfaces. This preliminary investigation demonstrated the potential of fluorescence imaging techniques for detection of biofilms on leafy green surfaces.
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Monitoring Insulin Aggregation via Capillary Electrophoresis
Pryor, Elizabeth; Kotarek, Joseph A.; Moss, Melissa A.; Hestekin, Christa N.
2011-01-01
Early stages of insulin aggregation, which involve the transient formation of oligomeric aggregates, are an important aspect in the progression of Type II diabetes and in the quality control of pharmaceutical insulin production. This study is the first to utilize capillary electrophoresis (CE) with ultraviolet (UV) detection to monitor insulin oligomer formation at pH 8.0 and physiological ionic strength. The lag time to formation of the first detected species in the aggregation process was evaluated by UV-CE and thioflavin T (ThT) binding for salt concentrations from 100 mM to 250 mM. UV-CE had a significantly shorter (5–8 h) lag time than ThT binding (15–19 h). In addition, the lag time to detection of the first aggregated species via UV-CE was unaffected by salt concentration, while a trend toward an increased lag time with increased salt concentration was observed with ThT binding. This result indicates that solution ionic strength impacts early stages of aggregation and β-sheet aggregate formation differently. To observe whether CE may be applied for the analysis of biological samples containing low insulin concentrations, the limit of detection using UV and laser induced fluorescence (LIF) detection modes was determined. The limit of detection using LIF-CE, 48.4 pM, was lower than the physiological insulin concentration, verifying the utility of this technique for monitoring biological samples. LIF-CE was subsequently used to analyze the time course for fluorescein isothiocyanate (FITC)-labeled insulin oligomer formation. This study is the first to report that the FITC label prevented incorporation of insulin into oligomers, cautioning against the use of this fluorescent label as a tag for following early stages of insulin aggregation. PMID:22272138
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NASA Astrophysics Data System (ADS)
Khezri, Somayeh; Bahram, Morteza; Samadi, Naser
2018-01-01
In this paper, we describe a rapid, low-cost and highly sensitive colorimetric method for the detection of isoprenaline, based on 2-amino-5-mercapto-1,3,4-thiadiazol (AMTD) functionalized gold nanoparticles (AMTD-AuNPs) as a sensing element. Hydrogen bonding interaction between isoprenaline and AMTD resulted in the aggregation of AuNPs and a consequent color change of AuNPs from red to blue. The concentration of isoprenaline could be detected with the naked eye or a UV-visible spectrometer. Results showed that the absorbance ratio (A650/A524) was linear with isoprenaline concentrations in the range of 0.2 to 2.6 μM (R = 0.997). The detection limit of this method was 0.08 μM. The proposed method is simple, without using complicated instruments and adding salts for enhancing sensitivity. This probe could be successfully applied to the determination of isoprenaline in human serum samples and urine samples after deproteinization.
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NASA Astrophysics Data System (ADS)
Sahoo, Amaresh Kumar; Sharma, Shilpa; Chattopadhyay, Arun; Ghosh, Siddhartha Sankar
2012-02-01
Rapid, simple and sensitive detection of bacterial contamination is critical for safeguarding public health and the environment. Herein, we report an easy method of detection as well as enumeration of the bacterial cell number on the basis of fluorescence quenching of a non-antibacterial fluorescent nanocomposite, consisting of paracetamol dimer (PD) and Au nanoparticles (NPs), in the presence of bacteria. The composite was synthesized by reaction of paracetamol (p-hydroxyacetanilide) with HAuCl4. The Au NPs of the composite were characterized using UV-Vis spectroscopy, transmission electron microscopy (TEM), X-ray diffraction and selected area electron diffraction analysis. The paracetamol dimer in the composite showed emission peak at 435 nm when excited at 320 nm. The method successfully detected six bacterial strains with a sensitivity of 100 CFU mL-1. The Gram-positive and Gram-negative bacteria quenched the fluorescence of the composite differently, making it possible to distinguish between the two. The TEM analysis showed interaction of the composite with bacteria without any apparent damage to the bacteria. The chi-square test established the accuracy of the method. Quick, non-specific and highly sensitive detection of bacteria over a broad range of logarithmic dilutions within a short span of time demonstrates the potential of this method as an alternative to conventional methods.Rapid, simple and sensitive detection of bacterial contamination is critical for safeguarding public health and the environment. Herein, we report an easy method of detection as well as enumeration of the bacterial cell number on the basis of fluorescence quenching of a non-antibacterial fluorescent nanocomposite, consisting of paracetamol dimer (PD) and Au nanoparticles (NPs), in the presence of bacteria. The composite was synthesized by reaction of paracetamol (p-hydroxyacetanilide) with HAuCl4. The Au NPs of the composite were characterized using UV-Vis spectroscopy, transmission electron microscopy (TEM), X-ray diffraction and selected area electron diffraction analysis. The paracetamol dimer in the composite showed emission peak at 435 nm when excited at 320 nm. The method successfully detected six bacterial strains with a sensitivity of 100 CFU mL-1. The Gram-positive and Gram-negative bacteria quenched the fluorescence of the composite differently, making it possible to distinguish between the two. The TEM analysis showed interaction of the composite with bacteria without any apparent damage to the bacteria. The chi-square test established the accuracy of the method. Quick, non-specific and highly sensitive detection of bacteria over a broad range of logarithmic dilutions within a short span of time demonstrates the potential of this method as an alternative to conventional methods. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr11837h
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Synthesis of ZnO nanopencils using wet chemical method and its investigation as LPG sensor
NASA Astrophysics Data System (ADS)
Shimpi, Navinchandra G.; Jain, Shilpa; Karmakar, Narayan; Shah, Akshara; Kothari, D. C.; Mishra, Satyendra
2016-12-01
ZnO nanopencils (NPCs) were prepared by a novel wet chemical process, using triethanolamine (TEA) as a mild base, which is relatively simple and cost effective method as compared to hydrothermal method. ZnO NPCs were characterized using powder X-ray diffraction (XRD), Fourier Transform Infra-Red (FTIR) spectroscopy in mid-IR and far-IR regions, X-ray Photoelectron Spectroscopy (XPS), UV-vis (UV-vis) absorption spectroscopy, room temperature Photoluminescence (PL) spectroscopy and Field Emission Scanning Electron Microscopy (FESEM). ZnO NPCs obtained, were highly pure, uniform and monodispersed.XRD pattern indicated hexagonal unit cell structure with preferred orientation along the c-axis. Sensing behaviour of ZnO NPCs was studied towards Liquefied Petroleum Gas (LPG) at different operating temperatures. The study shows that ZnO NPCs were most sensitive and promising candidate for detection of LPG at 250 °C with gas sensitivity > 60%. The high response towards LPG is due to high surface area of ZnO NPCs and their parallel alignment.
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Bodai, Zsolt; Szabó, Bálint Sámuel; Novák, Márton; Hámori, Susanne; Nyiri, Zoltán; Rikker, Tamás; Eke, Zsuzsanna
2014-10-15
A simple and fast analytical method was developed for the determination of six UV stabilizers (Cyasorb UV-1164, Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, and Tinuvin 1577) and five antioxidants (Irgafos 168, Irganox 1010, Irganox 3114, Irganox 3790, and Irganox 565) in milk. For sample preparation liquid-liquid extraction with low-temperature purification combined with centrifugation was used to remove fats, proteins, and sugars. After the cleanup step, the sample was analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). External standard and matrix calibrations were tested. External calibration proved to be acceptable for Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, Irganox 3114, and Irganox 3790. The method was successfully validated with matrix calibration for all compounds. Method detection limits were between 0.25 and 10 μg/kg. Accuracies ranged from 93 to 109%, and intraday precisions were <13%.
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Kheyrandish, Ataollah; Mohseni, Madjid; Taghipour, Fariborz
2018-06-15
Determining fluence is essential to derive the inactivation kinetics of microorganisms and to design ultraviolet (UV) reactors for water disinfection. UV light emitting diodes (UV-LEDs) are emerging UV sources with various advantages compared to conventional UV lamps. Unlike conventional mercury lamps, no standard method is available to determine the average fluence of the UV-LEDs, and conventional methods used to determine the fluence for UV mercury lamps are not applicable to UV-LEDs due to the relatively low power output, polychromatic wavelength, and specific radiation profile of UV-LEDs. In this study, a method was developed to determine the average fluence inside a water suspension in a UV-LED experimental setup. In this method, the average fluence was estimated by measuring the irradiance at a few points for a collimated and uniform radiation on a Petri dish surface. New correction parameters were defined and proposed, and several of the existing parameters for determining the fluence of the UV mercury lamp apparatus were revised to measure and quantify the collimation and uniformity of the radiation. To study the effect of polychromatic output and radiation profile of the UV-LEDs, two UV-LEDs with peak wavelengths of 262 and 275 nm and different radiation profiles were selected as the representatives of typical UV-LEDs applied to microbial inactivation. The proper setup configuration for microorganism inactivation studies was also determined based on the defined correction factors.
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Beacons into the Cosmic Dark Ages: Boosted Transmission of Lyα from UV Bright Galaxies at z ≳ 7
NASA Astrophysics Data System (ADS)
Mason, Charlotte A.; Treu, Tommaso; de Barros, Stephane; Dijkstra, Mark; Fontana, Adriano; Mesinger, Andrei; Pentericci, Laura; Trenti, Michele; Vanzella, Eros
2018-04-01
Recent detections of Lyman alpha (Lyα) emission from z > 7.5 galaxies were somewhat unexpected given a dearth of previous non-detections in this era when the intergalactic medium (IGM) is still highly neutral. But these detections were from UV bright galaxies, which preferentially live in overdensities that reionize early, and have significantly Doppler-shifted Lyα line profiles emerging from their interstellar media (ISM), making them less affected by the global IGM state. Using a combination of reionization simulations and empirical ISM models we show, as a result of these two effects, that UV bright galaxies in overdensities have >2× higher transmission through the z ∼ 7 IGM than typical field galaxies, and that this boosted transmission is enhanced as the neutral fraction increases. The boosted transmission is not sufficient to explain the observed high Lyα fraction of M UV ≲ ‑22 galaxies, suggesting that Lyα emitted by these galaxies must be stronger than expected due to enhanced production and/or selection effects. Despite the bias of UV bright galaxies to reside in overdensities we show Lyα observations of such galaxies can accurately measure the global neutral hydrogen fraction, particularly when Lyα from UV faint galaxies is extinguished, making them ideal candidates for spectroscopic follow-up into the cosmic Dark Ages.
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Luteolin as reactive oxygen generator by X-ray and UV irradiation
NASA Astrophysics Data System (ADS)
Toyama, Michiru; Mori, Takashi; Takahashi, Junko; Iwahashi, Hitoshi
2018-05-01
Non-toxic X-ray-responsive substances can be used in the radiosensitization of cancer, like porphyrin mediated radiotherapy. However, most X-ray-responsive substances are toxic. To find novel non-toxic X-ray-responsive substances, we studied the X-ray and UV reactivity of 40 non-toxic compounds extracted from plants. Dihydroethidium was used as an indicator to detect reactive oxygen species (ROS) generated by the compounds under X-ray or UV irradiation. We found that 13 of the investigated compounds generated ROS under X-ray irradiation and 17 generated ROS under UV irradiation. Only 4 substances generated ROS under both X-ray and UV. In particular, luteolin exhibited the highest activity among the investigated compounds; therefore, the ROS generated by luteolin were thoroughly characterized. To identify the ROS, we employed a combination of ROS detection reagents and their quenchers. O2·- generation by luteolin was monitored using dihydroethidium and superoxide dismutase (as an O2·- quencher). OH· and 1O2 generation was determined using aminophenyl fluorescein with ethanol (OH· quencher) and Singlet Oxygen Sensor Green® with NaN3 (1O2 quencher), respectively. Generation of O2·- under X-ray and UV irradiation was observed; however, no OH· or 1O2 was detected. The production of ROS from luteolin is surprising, because luteolin is a well-known antioxidant.
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Charehsaz, Mohammad; Gürbay, Aylin; Aydin, Ahmet; Sahin, Gönül
2014-01-01
In this study, a high-performance liquid chromatographic method (HPLC) and UV spectrophotometric method were developed, validated and applied for the determination of theophylline in biological fluids. Liquid- liquid extraction is performed for isolation of the drug and elimination of plasma and saliva interferences. Urine samples were applied without any extraction. The chromatographic separation was achieved on a C18 column by using 60:40 methanol:water as mobile phase under isocratic conditions at a flow rate of 0.75 mL/min with UV detection at 280 nm in HPLC method. UV spectrophotometric analysis was performed at 275 nm. the limit of quantification: 1.1 µg/mL for urine, 1.9 µg/mL for saliva, 3.1 µg/mL for plasma; recovery: 94.85% for plasma, 100.45% for saliva, 101.39% for urine; intra-day precision: 0.22-2.33%, inter-day precision: 3.17-13.12%. Spectrophotometric analysis results were as follows: the limit of quantitation: 5.23 µg/mL for plasma, 8.7 µg/mL for urine; recovery: 98.27% for plasma, 95.25% for urine; intra-day precision: 2.37 - 3.00%, inter-day precision: 5.43-7.91%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of theophylline in biological samples. Also spectrophotometric analysis can be used where it can be applicable.
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Chen, Xiao; Wan, Yanjian; Chen, Xi; Li, Yuanyuan
2018-01-01
2,4-Dichlorophenoxyacetic acid (2,4-D) is a chlorophenoxy herbicide used worldwide. We describe a high-performance liquid chromatography (HPLC) method with UV detection for the determination of 2,4-D in female and male rat serum. This allows to observe the change of serum 2,4-D concentration in rats with time and its pharmacokinetics characteristics with a simple, rapid, optimized and validated method. The serum samples are pretreated and introduced into the HPLC system. The analytes are separated in a XDB-C18 column with a mobile phase of acetonitrile (solvent A) and 0.02 M ammonium acetate (containing 0.1% formic acid) (solvent B) using a gradient elution at a flow rate of 1.0 mL/min. The wavelength for UV detection was set at 230 nm. Calibration curve for 2,4-D was constructed over a range of 0.1–400 mg/L. The method was successfully applied to study the pharmacokinetics of 2,4-D in rats in this study. After oral administration of 300 mg/kg and 60 mg/kg 2,4-D, the mean Cmax values were 601.9 and 218.4 mg/L, the AUC0→∞ values were 23,722 and 4,127 mg×h/L and the clearance (Cl) were 1.10 and 0.02 L/(h×kg), respectively. The developed method was found to be specific, precise, reproducible and rapid. PMID:29342170
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Chen, Xiao; Zhang, Hongling; Wan, Yanjian; Chen, Xi; Li, Yuanyuan
2018-01-01
2,4-Dichlorophenoxyacetic acid (2,4-D) is a chlorophenoxy herbicide used worldwide. We describe a high-performance liquid chromatography (HPLC) method with UV detection for the determination of 2,4-D in female and male rat serum. This allows to observe the change of serum 2,4-D concentration in rats with time and its pharmacokinetics characteristics with a simple, rapid, optimized and validated method. The serum samples are pretreated and introduced into the HPLC system. The analytes are separated in a XDB-C18 column with a mobile phase of acetonitrile (solvent A) and 0.02 M ammonium acetate (containing 0.1% formic acid) (solvent B) using a gradient elution at a flow rate of 1.0 mL/min. The wavelength for UV detection was set at 230 nm. Calibration curve for 2,4-D was constructed over a range of 0.1-400 mg/L. The method was successfully applied to study the pharmacokinetics of 2,4-D in rats in this study. After oral administration of 300 mg/kg and 60 mg/kg 2,4-D, the mean Cmax values were 601.9 and 218.4 mg/L, the AUC0→∞ values were 23,722 and 4,127 mg×h/L and the clearance (Cl) were 1.10 and 0.02 L/(h×kg), respectively. The developed method was found to be specific, precise, reproducible and rapid.
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NASA Astrophysics Data System (ADS)
Šojić, D.; Despotović, V.; Orčić, D.; Szabó, E.; Arany, E.; Armaković, S.; Illés, E.; Gajda-Schrantz, K.; Dombi, A.; Alapi, T.; Sajben-Nagy, E.; Palágyi, A.; Vágvölgyi, Cs.; Manczinger, L.; Bjelica, L.; Abramović, B.
2012-11-01
SummaryA comprehensive study of the degradation of thiamethoxam (THIA) and metoprolol (MET) was conducted by using UV-induced photolysis (λ = 254 nm), ozonation, and a combination of these methods. In order to investigate how molecular structure of the substrate influences the rate of its degradation, we compared these three processes for the insecticide THIA and the drug MET (a β1-blocker). Of the three treatments applied, the UV photolysis and the combination of UV/O3 were found to be most effective in the degradation of THIA, while the UV/O3 process appeared to be the most efficient in terms of MET decay. The degradation kinetics was monitored by LC-DAD, and spectrophotometry, while the mineralization of the substrates was studied by TOC analysis. Reaction intermediates were studied in detail and a number of them were identified using LC-MS (ESI+/ESI-). Both parent compounds showed slight toxic effects towards algae Pseudokirchneriella subcapitata and bacteria Vibrio fischeri. However, the toxicity of the solutions containing also the degradation intermediates appeared to be much higher for all the test organisms. The inhibition/mortality rates were reduced most efficiently by the UV/O3 procedure. Ames test and Comet assay were used to follow the genotoxicity during the degradation of the studied compounds. Genotoxic intermediates were frequently detected in the case of MET in the UV treatment alone or in the presence of ozone. Treatments of THIA samples resulted less frequently in genotoxic intermediates. To our best knowledge, this work is the first genotoxicological investigation dealing with the photolytic degradation process of the studied compounds.
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Wako, Hiromichi; Ishiuchi, Shun-Ichi; Kato, Daichi; Féraud, Géraldine; Dedonder-Lardeux, Claude; Jouvet, Christophe; Fujii, Masaaki
2017-05-03
The conformer-selected ultraviolet (UV) and infrared (IR) spectra of protonated noradrenaline were measured using an electrospray/cryogenic ion trap technique combined with photo-dissociation spectroscopy. By comparing the UV photo dissociation (UVPD) spectra with the UV-UV hole burning (HB) spectra, it was found that five conformers coexist under ultra-cold conditions. Based on the spectral features of the IR dip spectra of each conformer, two different conformations on the amine side chain were identified. Three conformers (group I) were assigned to folded and others (group II) to extended structures by comparing the observed IR spectra with the calculated ones. Observation of the significantly less-stable extended conformers strongly suggests that the extended structures are dominant in solution and are detected in the gas phase by kinetic trapping. The conformers in each group are assignable to rotamers of OH orientations in the catechol ring. By comparing the UV-UV HB spectra and the calculated Franck-Condon spectra obtained by harmonic vibrational analysis of the S 1 state, with the aid of relative stabilization energies of each conformer in the S 0 state, the absolute orientations of catechol OHs of the observed five conformers were successfully determined. It was found that the 0-0 transition of one folded conformer is red-shifted by about 1000 cm -1 from the others. The significant red-shift was explained by a large contribution of the πσ* state to S 1 in the conformer in which an oxygen atom of the meta-OH group is close to the ammonium group.
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Fedenko, Volodymyr S; Shemet, Sergiy A; Landi, Marco
2017-05-01
Although anthocyanin (ACN) biosynthesis is one of the best studied pathways of secondary metabolism in plants, the possible physiological and ecological role(s) of these pigments continue to intrigue scientists. Like other dihydroxy B-ring substituted flavonoids, ACNs have an ability to bind metal and metalloid ions, a property that has been exploited for a variety of purposes. For example, the metal binding ability may be used to stabilize ACNs from plant food sources, or to modify their colors for using them as food colorants. The complexation of metals with cyanidin derivatives can also be used as a simple, sensitive, cheap, and rapid method for determination concentrations of several metals in biological and environmental samples using UV-vis spectroscopy. Far less information is available on the ecological significance of ACN-metal complexes in plant-environment interactions. Metalloanthocyanins (protocyanin, nemophilin, commelinin, protodelphin, cyanosalvianin) are involved in the copigmentation phenomenon that leads to blue-pigmented petals, which may facilitate specific plant-pollinator interactions. ACN-metal formation and compartmentation into the vacuole has also been proposed to be part of an orchestrated detoxification mechanism in plants which experience metal/metalloid excess. However, investigations into ACN-metal interactions in plant biology may be limited because of the complexity of the analytical techniques required. To address this concern, here we describe simple methods for the detection of ACN-metal both in vitro and in vivo using UV-vis spectroscopy and colorimetric models. In particular, the use of UV-vis spectra, difference absorption spectra, and colorimetry techniques will be described for in vitro determination of ACN-metal features, whereas reflectance spectroscopy and colorimetric parameters related to CIE L * a * b * and CIE XYZ systems will be detailed for in vivo analyses. In this way, we hope to make this high-informative tool more accessible to plant physiologists and ecologists. Copyright © 2017 Elsevier GmbH. All rights reserved.
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Hähnel, Viola; Dormann, Frauke; Nitsopoulos, Athanasios; Friedle, Albrecht; Ahrens, Norbert
2017-02-15
Extracorporeal photopheresis (ECP) is an efficient method to treat various autoimmune diseases, cutaneous T-cell lymphoma, and graft-versus-host disease. It is based on the ex vivo inactivation of lymphocytes by 8-methoxypsoralen (8-MOP)/UV light treatment. Despite the adhesive, lipophilic nature of 8-MOP, no quality control is established for the ECP procedure. We developed a sensitive high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) assay to monitor residual 8-MOP concentration after UVA irradiation in the whole blood supernatant after acetonitrile precipitation. The preanalytical stability of 8-MOP exceeded 7 days, allowing batch mode analysis. Linearity was determined with R 2 above 0.99. The 8-MOP concentrations decreased exponentially after UV exposure, with decay constants of 0.0259 in plasma and 0.0528 in saline. The recovery of 8-MOP in photopheresates was about 68%, indicating binding to DNA as well as to plastic structures. UVA induced no 8-MOP fragmentation, but caused self-adducts under extreme conditions (10-fold UV dosage). Detection of 8-MOP proved to be feasible and demonstrated that the doses were in the pharmaceutically active range.
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Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E
2015-09-01
An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. Copyright © 2015. Published by Elsevier B.V.
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Quality of Rapeseed Bio-Fuel Waste: Optical Properties
NASA Astrophysics Data System (ADS)
Sujak, Agnieszka; Muszyñski, Siemowit; Kachel-Jakubowska, Magdalena
2014-04-01
The objective of the presented work was to examine the optical properties of selected bio-fuel waste. Three independent optical methods: UV-Vis spectroscopy, infrared spectroscopy and chromametric measurements were applied to establish the possible quality control test for the obtained substances. The following by-products were tested: distilled glycerine, technical glycerine and matter organic non glycerine fraction from rapeseed oil bio-fuel production. The results show that analysis of UV-Vis spectra can give rapid information about the purity of distilled glycerine, while no direct information can be obtained concerning the concentration and kind of impurities. Transmission mode is more useful as compared to absorption, concerning the detection abilities of average UV-Vis spectrometers. Infrared spectroscopy can be used as a complementary method for determining impurities/admixtures in samples. Measurements of chroma give the quickest data to compare the colour of biofuel by-products obtained by different producers. The condition is, however, that the products are received through the same or similar chemical processes. The other important factor is application of well defined measuring background. All the discussed analyses are quick, cheap and non-destructive, and can help to compare the quality of products.
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Design of electrostatically levitated micromachined rotational gyroscope based on UV-LIGA technology
NASA Astrophysics Data System (ADS)
Cui, Feng; Chen, Wenyuan; Su, Yufeng; Zhang, Weiping; Zhao, Xiaolin
2004-12-01
The prevailing micromachined vibratory gyroscope typically has a proof mass connected to the substrate by a mechanical suspension system, which makes it face a tough challenge to achieve tactical or inertial grade performance levels. With a levitated rotor as the proof mass, a micromachined rotational gyroscope will potentially have higher performance than vibratory gyroscope. Besides working as a moment rebalance dual-axis gyroscope, the micromachined rotational gyroscope based on a levitated rotor can simultaneously work as a force balance tri-axis accelerometer. Micromachined rotational gyroscope based on an electrostatically levitated silicon micromachined rotor has been notably developed. In this paper, factors in designing a rotational gyro/accelerometer based on an electrostatically levitated disc-like rotor, including gyroscopic action of micro rotor, methods of stable levitation, micro displacement detection and control, rotation drive and speed control, vacuum packaging and microfabrication, are comprehensively considered. Hence a design of rotational gyro/accelerometer with an electroforming nickel rotor employing low cost UV-LIGA technology is presented. In this design, a wheel-like flat rotor is proposed and its basic dimensions, diameter and thickness, are estimated according to the required loading capability. Finally, its micromachining methods based on UV-LIGA technology and assembly technology are discussed.
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Zhu, Hai-Zhen; Liu, Wei; Mao, Jian-Wei; Yang, Ming-Min
2008-04-28
4-Amino-4'-nitrobiphenyl, which is formed by catalytic effect of trichlorfon on sodium perborate oxidizing benzidine, is extracted with a cloud point extraction method and then detected using a high performance liquid chromatography with ultraviolet detection (HPLC-UV). Under the optimum experimental conditions, there was a linear relationship between trichlorfon in the concentration range of 0.01-0.2 mgL(-1) and the peak areas of 4-amino-4'-nitrobiphenyl (r=0.996). Limit of detection was 2.0 microgL(-1), recoveries of spiked water and cabbage samples ranged between 95.4-103 and 85.2-91.2%, respectively. It was proved that the cloud point extraction (CPE) method was simple, cheap, and environment friendly than extraction with organic solvents and had more effective extraction yield.