Development of liquid chromatographic methods for the determination of phytosterols in Standard Reference Materials containing saw palmetto.

Science.gov (United States)

Bedner, Mary; Schantz, Michele M; Sander, Lane C; Sharpless, Katherine E

2008-05-23

Liquid chromatographic (LC) methods using atmospheric pressure chemical ionization/mass spectrometric (APCI-MS) detection were developed for the separation and analysis of the phytosterols campesterol, cycloartenol, lupenone, lupeol, beta-sitosterol, and stigmasterol. Brassicasterol and cholesterol were also included for investigation as internal standards. The methods were used to identify and quantify the phytosterols in each of two Serenoa repens (saw palmetto) Standard Reference Materials (SRMs) developed by the National Institute of Standards and Technology (NIST). Values obtained by LC-MS were compared to those obtained using the more traditional approach of gas chromatography with flame ionization detection. This is the first reported use of LC-MS to determine phytosterols in saw palmetto dietary supplement materials.

Preparation and analysis of standardized waste samples for Controlled Ecological Life Support Systems (CELSS)

Science.gov (United States)

Carden, J. L.; Browner, R.

1982-01-01

The preparation and analysis of standardized waste samples for controlled ecological life support systems (CELSS) are considered. Analysis of samples from wet oxidation experiments, the development of ion chromatographic techniques utilizing conventional high pressure liquid chromatography (HPLC) equipment, and an investigation of techniques for interfacing an ion chromatograph (IC) with an inductively coupled plasma optical emission spectrometer (ICPOES) are discussed.

Gas chromatographic determination of Di-n-butyl phosphate in radioactive lean organic solvent of FBTR carbide fuel reprocessing

International Nuclear Information System (INIS)

Velavendan, P.; Ganesh, S.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

2011-01-01

In the present work Di-n- butyl phosphate (DBP) a degraded product of Tri-n-butyl phosphate (TBP) formed by acid hydrolysis and radiolysis in the PUREX process was analyzed. Lean organic streams of different fuel burn-up FBTR carbide fuel reprocessing solution was determined by standard Gas Chromatographic technique. The method involves the conversion of non-volatile Di-n-butyl phosphate into volatile and stable derivatives by the action of diazomethane and then determined by Gas Chromatograph (GC). A calibration graph was made for DBP concentration range of 200-2000 ppm with correlation coefficient of 0.99587 and RSD 1.2 %. (author)

A high-throughput headspace gas chromatographic technique for the determination of nitrite content in water samples.

Science.gov (United States)

Zhang, Shu-Xin; Peng, Rong; Jiang, Ran; Chai, Xin-Sheng; Barnes, Donald G

2018-02-23

This paper reports on a high-throughput headspace gas chromatographic method (HS-GC) for the determination of nitrite content in water sample, based on GC measurement of cyclohexene produced from the reaction between nitrite and cyclamate in a closed vial. The method has a relative standard deviation of water samples. In short, the present HS-GC method is simple, accurate, and sensitive, and it is very suitable to be used in the batch sample testing. Copyright © 2018 Elsevier B.V. All rights reserved.

Probabilistic peak detection for first-order chromatographic data.

Science.gov (United States)

Lopatka, M; Vivó-Truyols, G; Sjerps, M J

2014-03-19

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by such a peak. The algorithm makes use of chromatographic information (i.e. the expected width of a single peak and the standard deviation of baseline noise). As prior information of the existence of a peak in a chromatographic run, we make use of the statistical overlap theory. We formulate an exhaustive set of mutually exclusive hypotheses concerning presence or absence of different peak configurations. These models are evaluated by fitting a segment of chromatographic data by least-squares. The evaluation of these competing hypotheses can be performed as a Bayesian inferential task. We outline the potential advantages of adopting this approach for peak detection and provide several examples of both improved performance and increased flexibility afforded by our approach. Copyright © 2014 Elsevier B.V. All rights reserved.

Isolation of Triterpenoid Glycoside from Bark of Terminalia arjuna using Chromatographic Technique and Investigation of Pharmacological Behavior upon Muscle Tissues

Directory of Open Access Journals (Sweden)

Tanushree Patnaik

2007-01-01

Full Text Available This study reports the isolation and characterization of a new triterpenoid glycoside extracted from the bark of Terminalia arjuna. The isolation of the organic compounds was done using simple chromatographic technique. Compound characterization using various spectroscopic technique identify the final isolated compound as Olean-3β,22β-diol-12-en-28β-D-glucopyranoside-oic acid. The method of isolation is simple, cost effective and efficient. The preliminary bioactivity of the compound was also evaluated.

Radioimmunoassay of methaqualone in human urine compared with chromatographic methods

International Nuclear Information System (INIS)

Mule, S.J.; Kogan, M.; Jukofsky, D.

1978-01-01

The 125 I-radioimmunoassay for methaqualone in human urine was evaluated by a comparison with newly modified gas-liquid chromatographic and thin-layer chromatographic methods. The statistically significant sensitivity value for the radioimmunoassay was at 2 μg of methaqualone per liter of urine. The coefficient of variation was 2.88 -+ 0.16% intraassay. There was cross-reactivity only with metabolites of methaqualone, 4'-hydroxymethaqualone being twice as sensitively measured as methaqualone. There was complete agreement between results by radioimmunoassay and by gas-liquid chromatography in 96.7% of the samples analyzed. Only 1.2% of the radioimmunoassay values were false positives, and 2.1% false negatives (phi = 0.8917, P < 0.001). Comparisons between the thin-layer chromatographic data and the gas--liquid chromatographic or radioimmunoassay data showed less agreement because of the 50- to 200-fold higher sensitivity of the latter techniques. Gas--liquid chromatography therefore appears to represent the best reference method for the evaluation of the radioimmunoassay, which appears to be a very sensitive and reliable technique for detecting methaqualone and its metabolites in human urine

Impurity analysis in EC-99mTC radiotracer using chromatographic techniques

International Nuclear Information System (INIS)

Almeida, E.V.; Fukumori, N.T.O.; Mengatti, J.; Silva, C.P.G.; Matsuda, M.M.N.

2008-01-01

The objective of this study was to develop two chromatographic methods of impurity analysis in radiotracer 99m Tc-EC: the Thin Layer Chromatography (TLC) and the High Performance Liquid Chromatography Reversed Phase (HPLC-RP)

Qualification of an Agilent Technologies 7890A gas chromatograph used in the biotechnology industry

International Nuclear Information System (INIS)

Alvarez Gonzalez, Alberto; Tambara Hernandez, Yanet; Alvarez Gil, Felix

2014-01-01

The drug manufacture is governed by strict international standards that guarantee reproducibility and consistency of results. The qualification of the instruments used in the productive processes, as well as in the characterization of products and their quality control are prerequisites to the validation of any analytical technique using them. One of the instrumental techniques used in the biotechnical industry is Gas Chromatography. A standard of pure caffeine was used for analysis in addition to a HP-5 30 m x 0,32 mm d.i. and 0,33 μm thick film column was used in a Gas Chromatograph coupled with a Flame Ionization Detector. For the testing of the different modules involved in the analysis (injector, column, oven and detector), an experimental design was made to estimate several parameters

Development, modelling, optimisation and scale-up of chromatographic purification of a therapeutic protein

DEFF Research Database (Denmark)

Mollerup, Jørgen; Hansen, Thomas Budde; Kidal, Steffen

2007-01-01

Development of a chromatographic purification step proceeds through a number of stages. High-throughput screening techniques are used to identify suitable resins. This technique is also suitable for the design of a capture step and some intermediate chromatographic steps, but development and true...... by industry. The theory of residence time based scale-up is developed and applied. (c) 2007 Elsevier B.V. All rights reserved....

Secretory immunoglobulin purification from whey by chromatographic techniques.

Science.gov (United States)

Matlschweiger, Alexander; Engelmaier, Hannah; Himmler, Gottfried; Hahn, Rainer

2017-08-15

Secretory immunoglobulins (SIg) are a major fraction of the mucosal immune system and represent potential drug candidates. So far, platform technologies for their purification do not exist. SIg from animal whey was used as a model to develop a simple, efficient and potentially generic chromatographic purification process. Several chromatographic stationary phases were tested. A combination of two anion-exchange steps resulted in the highest purity. The key step was the use of a small-porous anion exchanger operated in flow-through mode. Diffusion of SIg into the resin particles was significantly hindered, while the main impurities, IgG and serum albumin, were bound. In this step, initial purity was increased from 66% to 89% with a step yield of 88%. In a second anion-exchange step using giga-porous material, SIg was captured and purified by step or linear gradient elution to obtain fractions with purities >95%. For the step gradient elution step yield of highly pure SIg was 54%. Elution of SIgA and SIgM with a linear gradient resulted in a step yield of 56% and 35%, respectively. Overall yields for both anion exchange steps were 43% for the combination of flow-through and step elution mode. Combination of flow-through and linear gradient elution mode resulted in a yield of 44% for SIgA and 39% for SIgM. The proposed process allows the purification of biologically active SIg from animal whey in preparative scale. For future applications, the process can easily be adopted for purification of recombinant secretory immunoglobulin species. Copyright © 2017 Elsevier B.V. All rights reserved.

Alternative chromatographic system for the quality control of lipophilic technetium-99m radiopharmaceuticals such as [99mTc(MIBI6]+

Directory of Open Access Journals (Sweden)

D.P. Faria

2015-01-01

Full Text Available Knowledge of the radiochemical purity of radiopharmaceuticals is mandatory and can be evaluated by several methods and techniques. Planar chromatography is the technique normally employed in nuclear medicine since it is simple, rapid and usually of low cost. There is no standard system for the chromatographic technique, but price, separation efficiency and short time for execution must be considered. We have studied an alternative system using common chromatographic stationary phase and alcohol or alcohol:chloroform mixtures as the mobile phase, using the lipophilic radiopharmaceutical [99mTc(MIBI6]+ as a model. Whatman 1 modified phase paper and absolute ethanol, Whatman 1 paper and methanol:chloroform (25:75, Whatman 3MM paper and ethanol:chloroform (25:75, and the more expensive ITLC-SG and 1-propanol:chloroform (10:90 were suitable systems for the direct determination of radiochemical purity of [99mTc(MIBI6]+ since impurities such as 99mTc-reduced-hydrolyzed (RH, 99mTcO4 - and [99mTc(cysteine2]- complex were completely separated from the radiopharmaceutical, which moved toward the front of chromatographic systems while impurities were retained at the origin. The time required for analysis was 4 to 15 min, which is appropriate for nuclear medicine routines.

Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

Science.gov (United States)

Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

2014-09-12

Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

Dual liquid and gas chromatograph system

Science.gov (United States)

Gay, D.D.

A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

Analytical method for the identification and assay of 12 phthalates in cosmetic products: application of the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques".

Science.gov (United States)

Gimeno, Pascal; Maggio, Annie-Françoise; Bousquet, Claudine; Quoirez, Audrey; Civade, Corinne; Bonnet, Pierre-Antoine

2012-08-31

Esters of phthalic acid, more commonly named phthalates, may be present in cosmetic products as ingredients or contaminants. Their presence as contaminant can be due to the manufacturing process, to raw materials used or to the migration of phthalates from packaging when plastic (polyvinyl chloride--PVC) is used. 8 phthalates (DBP, DEHP, BBP, DMEP, DnPP, DiPP, DPP, and DiBP), classified H360 or H361, are forbidden in cosmetics according to the European regulation on cosmetics 1223/2009. A GC/MS method was developed for the assay of 12 phthalates in cosmetics, including the 8 phthalates regulated. Analyses are carried out on a GC/MS system with electron impact ionization mode (EI). The separation of phthalates is obtained on a cross-linked 5%-phenyl/95%-dimethylpolysiloxane capillary column 30 m × 0.25 mm (i.d.) × 0.25 mm film thickness using a temperature gradient. Phthalate quantification is performed by external calibration using an internal standard. Validation elements obtained on standard solutions, highlight a satisfactory system conformity (resolution>1.5), a common quantification limit at 0.25 ng injected, an acceptable linearity between 0.5 μg mL⁻¹ and 5.0 μg mL⁻¹ as well as a precision and an accuracy in agreement with in-house specifications. Cosmetic samples ready for analytical injection are analyzed after a dilution in ethanol whereas more complex cosmetic matrices, like milks and creams, are assayed after a liquid/liquid extraction using ter-butyl methyl ether (TBME). Depending on the type of cosmetics analyzed, the common limits of quantification for the 12 phthalates were set at 0.5 or 2.5 μg g⁻¹. All samples were assayed using the analytical approach described in the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques". This analytical protocol is particularly adapted when it is not possible to make reconstituted sample matrices. Copyright © 2012

Use of adsorption and gas chromatographic techniques in estimating biodegradation of indigenous crude oils

International Nuclear Information System (INIS)

Kokub, D.; Allahi, A.; Shafeeq, M.; Khalid, Z.M.; Malik, K.A.; Hussain, A.

1993-01-01

Indigenous crude oils could be degraded and emulsified upto varying degree by locally isolated bacteria. Degradation and emulsification was found to be dependent upon the chemical composition of the crude oils. Tando Alum and Khashkheli crude oils were emulsified in 27 and 33 days of incubation respectively. While Joyamair crude oil and not emulsify even mainly due to high viscosity of this oil. Using adsorption chromatographic technique, oil from control (uninoculated) and bio degraded flasks was fractioned into the deasphaltened oil containing saturate, aromatic, NSO (nitrogen, sulphur, oxygen) containing hydrocarbons) and soluble asphaltenes. Saturate fractions from control and degraded oil were further analysed by gas liquid chromatography. From these analyses, it was observed that saturate fraction was preferentially utilized and the crude oils having greater contents of saturate fraction were better emulsified than those low in this fraction. Utilization of various fractions of crude oils was in the order saturate> aromatic> NSO. (author)

Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC

Directory of Open Access Journals (Sweden)

Nor Nasriah Zaini

2016-04-01

Full Text Available E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL−1 (r2 = 0.997 with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules. Selected chemometric techniques: cluster analysis (CA, discriminant analysis (DA, and principal component analysis (PCA were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

Spectrographic determination of lanthanides in high-purity uranium compounds, after chromatographic separation by alumina-hydrofluoric acid

International Nuclear Information System (INIS)

Lordello, A.R.; Abrao, A.

1979-01-01

A method is presented for the determination of fourteen rare earth elements in high-purity uranium compounds by emission spectrography. The rare earths are chromatographically separated from uranium by using alumina-hydrofluoric acid. Lanthanum is used both as collector and internal standard. The technique of excitation involves a total consumption of the sample in a 17 ampere direct current arc. The range of determination is about 0.005 to 0.5 μg/g uranium. The coefficient of variation for Pr, Ho, Dy, Er, Tm, Lu, Gd and Tb amounts to 10%. (Author) [pt

Alternative chromatographic system for the quality control of lipophilic technetium-99m radiopharmaceuticals such as [{sup 99m}Tc(MIBI){sub 6}]{sup +}

Energy Technology Data Exchange (ETDEWEB)

Faria, D.P.; Buchpiguel, C.A.; Marques, F.L.N., E-mail: danielefaria1@gmail.com [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil). Faculdade de Medicina. Departamento de Radiologia. Servico de Medicina Nuclear

2015-10-15

Knowledge of the radiochemical purity of radiopharmaceuticals is mandatory and can be evaluated by several methods and techniques. Planar chromatography is the technique normally employed in nuclear medicine since it is simple, rapid and usually of low cost. There is no standard system for the chromatographic technique, but price, separation efficiency and short time for execution must be considered. We have studied an alternative system using common chromatographic stationary phase and alcohol or alcohol:chloroform mixtures as the mobile phase, using the lipophilic radiopharmaceutical [{sup 99m}Tc(MIBI){sub 6}]{sup +} as a model. Whatman 1 modified phase paper and absolute ethanol, Whatman 1 paper and methanol: chloroform (25:75), Whatman 3MM paper and ethanol:chloroform (25:75), and the more expensive ITLC-SG and 1-propanol: chloroform (10:90) were suitable systems for the direct determination of radiochemical purity of [{sup 99m}Tc(MIBI){sub 6}]{sup +} since impurities such as {sup 99m}Tc-reduced-hydrolyzed (RH), {sup 99m}TcO4{sup -} and [{sup 99m}Tc(cysteine){sub 2}]{sup -} complex were completely separated from the radiopharmaceutical, which moved toward the front of chromatographic systems while impurities were retained at the origin. The time required for analysis was 4 to 15 min, which is appropriate for nuclear medicine routines. (author)

Methods of direct (non-chromatographic) quantification of body metabolites utilizing chemical ionization mass spectrometry

International Nuclear Information System (INIS)

Mee, J.M.L.

1978-01-01

For quantitative determination of known metabolites from the biological sample by direct chemical ionization mass spectrometry (CI-MS), the method of internal standard using stable isotopically labelled analogs appears to be the method of choice. In the case where stable isotope ratio determinations could not be applied, and alternative quantification can be achieved using non-labelled external or internal standards and a calibration curve (sum of peak height per a given number of scans versus concentration). The technique of computer monitoring permits display and plotting of ion current profiles (TIC and SIC) or spectra per a given number of scans or a given range of mass per charge. Examples are given in areas of clinical application and the quantitative data show very good agreement with the conventional chromatographic measurements. (Auth.)

Amalgam-chromatographic separation of magnesium isotopes

International Nuclear Information System (INIS)

Klinskij, G.D.; Levkin, A.V.; Ivanov, S.A.

1990-01-01

Separation of magnesium isotopes within Mg(Hg)-MgI 2 system (in dimethylformamide) is conducted under amalgam-chromatographic conditions. Separation maximal degree, that is (1.09), for 24 Mg and 26 Mg and separation coefficient (α = 1.0089±0.006) are determined. Light isotopes are found to concentrate in the amalgam. Technique of thermal conversion of flows within amalgam-dimethylformamide system is suggested on the basis of reversible reaction of Ca-Mg element exchange

Validation for chromatographic and electrophoretic methods

OpenAIRE

Ribani, Marcelo; Bottoli, Carla Beatriz Grespan; Collins, Carol H.; Jardim, Isabel Cristina Sales Fontes; Melo, Lúcio Flávio Costa

2004-01-01

The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the dif...

The gas-chromatographic and gas-chromatographic-mass-spectrometric identification of halogen-containing organic compounds

Science.gov (United States)

Gidaspov, B. V.; Zenkevich, I. G.; Rodin, A. A.

1989-09-01

The problem of identifying halogen-containing organic compounds in their gas-chromatographic and gas-chromatographic-mass-spectrometric (GC-MS) determination in different materials has been examined. Particular attention has been paid not to the complete characterisation of methods for carrying out this analysis but to the most important problem of increasing the selectivity at the stages of sampling, separation, and interpretation of the gas-chromatographic and GC-MS information. The bibliography contains 292 references.

Chromatographic determination of silicon and phosphorus as molybdic heteropoly acids with preconcentration

International Nuclear Information System (INIS)

Tikhomirova, T.I.; Krokhin, O.V.; Dubovik, D.B.; Ivanov, A.V.; Shpigun, O.A.

2002-01-01

Chromatographic behaviour of silicon and phosphorus as molybdic heteropoly acids with preconcentration as ion associations of heteropoly acid with tributylammonium bromide was studied. The technique of simultaneous analysis of silicon and phosphorus was developed. During investigation into the effect of acetonitril content in the probe on the form of chromatographic peak of molybdosilicic acid the negative influence of acetonitril on the form of peak was ascertained. This effect may be eliminated by the lowering of acetonitril content up to 50 %. It was found that under these conditions the chromatographic peak practically was absent, because of the heteropoly acid of the Mo(VI) abundance transformed in the MoO 2 2+ cation form without reaction with tributylammonium cation during concentration of heteropoly acid [ru

Characterization of spent nuclear fuels by an online combination of chromatographic and mass spectrometric techniques

International Nuclear Information System (INIS)

Guenther-Leopold, Ines; Wernli, Beat; Kopajtic, Zlatko

2003-01-01

The determination of the burn-up is one of the essential parts in post-irradiation examinations on nuclear fuel samples. In the frame of national and international research programs the analysis of the isotopic vectors of uranium, plutonium, neodymium and some other fission products and actinides was carried out in the Hot lab of the Paul Scherrer Institute in the last years by using high-performance liquid chromatography coupled online with an inductively coupled plasma quadrupole mass spectrometer. In the meantime a multicollector ICP-MS, suitable for high precision isotope ratio measurements, was installed within the Hot lab and has been used now in combination with a chromatographic separation system for the first time for burn-up determinations of nuclear fuel samples. The results of these investigations, a comparison of both methods with the classical technique for burn-up analyses (thermal ionization mass spectrometry), the advantages and limitations of the methods and the accuracy and precision of this type of analyses are presented in the paper. (author)

High Performance Liquid Chromatographic Method for Determination of Dipyridamole in Human Plasma

Directory of Open Access Journals (Sweden)

DAVOOD BEIGI BAND ARAB ADI

1999-08-01

Full Text Available A simple, rapid and specific high-performance liquid chromatographic procedure is reported for"nquantitative determination of dipyridamole in human -plasma. The assay uses a reversed-phase"nhigh-performance liquid chromatographic (HPLC and UV detection at 280nm and has a limit"nof detection of approximately 5ng/mL. The mobile phase consists of MeOH-H20 (60:40"nadjusted to pH 3.3. Dipyridamole was extracted from plasma by back-extraction procedure, with"npropranolol as the internal standard. The reproducibility of the method is satisfactory

[Ideas and methods of two-dimensional zebrafish model combined with chromatographic techniques in high-throughput screening of active anti-osteoporosis components of traditional Chinese medicines].

Science.gov (United States)

Wei, Ying-Jie; Jing, Li-Jun; Zhan, Yang; Sun, E; Jia, Xiao-Bin

2014-05-01

To break through the restrictions of the evaluation model and the quantity of compounds by using the two-dimensional zebrafish model combined with chromatographic techniques, and establish a new method for the high-throughput screening of active anti-osteoporosis components. According to the research group-related studies and relevant foreign literatures, on the basis of the fact that the zebrafish osteoporosis model could efficiently evaluate the activity, the zebrafish metabolism model could efficiently enrich metabolites and the chromatographic techniques could efficiently separate and analyze components of traditional Chinese medicines, we proposed that the inherent combination of the three methods is expected to efficiently decode in vivo and in vitro efficacious anti-osteoporosis materials of traditional Chinese medicines. The method makes it simple and efficient in the enrichment, separation and analysis on components of traditional Chinese medicines, particularly micro-components and metabolites and the screening anti-osteoporosis activity, fully reflects that efficacious materials of traditional Chinese medicines contain original components and metabolites, with characteristic of "multi-components, multi-targets and integral effect", which provides new ideas and methods for the early and rapid discovery of active anti-osteoporosis components of traditional Chinese medicines.

Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

1993-01-01

Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...... and dimethylarsinate and the cations arsenobetaine, trimethylarsine oxide, arsenocholine and the tetramethylarsonium ion. Hexahydroxyantimonate(III) was co-chromatographed with the arsenic anions but detected at m/z 121 and used as an internal standard for their qualitative analysis. Arsenite was prone to oxidation....... The argon chloride interference at m/z 75 was eliminated by chromatographic separation of the chloride present in the sample from the arsenic analytes. The ClO+ ion detected at m/z 51 and 53 was used to monitor the retention time of chloride in the anion-exchange system. The chloride eluted about 100 s...

[A peak recognition algorithm designed for chromatographic peaks of transformer oil].

Science.gov (United States)

Ou, Linjun; Cao, Jian

2014-09-01

In the field of the chromatographic peak identification of the transformer oil, the traditional first-order derivative requires slope threshold to achieve peak identification. In terms of its shortcomings of low automation and easy distortion, the first-order derivative method was improved by applying the moving average iterative method and the normalized analysis techniques to identify the peaks. Accurate identification of the chromatographic peaks was realized through using multiple iterations of the moving average of signal curves and square wave curves to determine the optimal value of the normalized peak identification parameters, combined with the absolute peak retention times and peak window. The experimental results show that this algorithm can accurately identify the peaks and is not sensitive to the noise, the chromatographic peak width or the peak shape changes. It has strong adaptability to meet the on-site requirements of online monitoring devices of dissolved gases in transformer oil.

Chromatographic fingerprinting through chemometric techniques for herbal slimming pills: A way of adulterant identification.

Science.gov (United States)

Shekari, Nafiseh; Vosough, Maryam; Tabar Heidar, Kourosh

2018-05-01

In the current study, gas chromatography-mass spectrometry (GC-MS) fingerprinting of herbal slimming pills assisted by chemometric methods has been presented. Deconvolution of two-way chromatographic signals of nine herbal slimming pills into pure chromatographic and spectral patterns was performed. The peak clusters were resolved using multivariate curve resolution-alternating least squares (MCR-ALS) by employing appropriate constraints. It was revealed that more useful chemical information about the composition of the slimming pills can be obtained by employing sophisticated GC-MS method coupled with proper chemometric tools yielding the extended number of identified constituents. The thorough fingerprinting of the complex mixtures proved the presence of some toxic or carcinogen components, such as toluene, furfural, furfuryl alcohol, styrene, itaconic anhydride, citraconic anhydride, trimethyl phosphate, phenol, pyrocatechol, p-propenylanisole and pyrogallol. In addition, some samples were shown to be adulterated with undeclared ingredients, including stimulants, anorexiant and laxatives such as phenolphthalein, amfepramone, caffeine and sibutramine. Copyright © 2018 Elsevier B.V. All rights reserved.

Modeling Aquatic Toxicity through Chromatographic Systems.

Science.gov (United States)

Fernández-Pumarega, Alejandro; Amézqueta, Susana; Farré, Sandra; Muñoz-Pascual, Laura; Abraham, Michael H; Fuguet, Elisabet; Rosés, Martí

2017-08-01

Environmental risk assessment requires information about the toxicity of the growing number of chemical products coming from different origins that can contaminate water and become toxicants to aquatic species or other living beings via the trophic chain. Direct toxicity measurements using sensitive aquatic species can be carried out but they may become expensive and ethically questionable. Literature refers to the use of chromatographic measurements that correlate to the toxic effect of a compound over a specific aquatic species as an alternative to get toxicity information. In this work, we have studied the similarity in the response of the toxicity to different species and we have selected eight representative aquatic species (including tadpoles, fish, water fleas, protozoan, and bacteria) with known nonspecific toxicity to chemical substances. Next, we have selected four chromatographic systems offering good perspectives for surrogation of the eight selected aquatic systems, and thus prediction of toxicity from the chromatographic measurement. Then toxicity has been correlated to the chromatographic retention factor. Satisfactory correlation results have been obtained to emulate toxicity in five of the selected aquatic species through some of the chromatographic systems. Other aquatic species with similar characteristics to these five representative ones could also be emulated by using the same chromatographic systems. The final aim of this study is to model chemical products toxicity to aquatic species by means of chromatographic systems to reduce in vivo testing.

Optimization of the gas chromatographic separations; Optimacion de las separaciones cromatograficas en fase gaseosa

Energy Technology Data Exchange (ETDEWEB)

Gasco Sanchez, L

1973-07-01

A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs.

Chromatographic determination of Terbinafine in presence of its Photodegradation products

International Nuclear Information System (INIS)

Abdel-Moety, E.M.; Kelani, K.O.; Abou Al-Alamein, A.M.

2003-01-01

Two different chromatographic techniques have been developed for the determination of terbinafine hydrochloride in presence of its photodegradation products. The first method depends on coupling the TLC- fractionation, on silicia gel 60F254 utilizing chloroform+methanol+25% aq. ammonia ( 12: 0.1:0.1,by volumes), with the direct scanning at 284nm. The second method describes a liquid chromatographic separation of terbinafine and its photolytic degradates on a reversed-phase column[u-Bondapak-TMC 18 (10um,25cmx4.6mm,i.d.)] using a mobile phase containing methanol+water= 80:20 (v/v) with UV-detection at 284 nm. The proposed methods showed significant stability-indication with good linearity, precision and reproducibility. (author)

Determination of SO2 in the atmosphere using radioactive iodine kryptonate as impregnation medium of chromatographic paper

International Nuclear Information System (INIS)

Pruzinec, J.

1975-01-01

Chromatographic paper was impregnated with radioiodine kryptonate using the macrodiffusion technique. The decrease with time of the activity of the kryptonate-impregnated paper exposed to SO 2 -contaminated air was measured. From the decrease in chromatographic paper activity, the concentration of SO 2 was determined in the range 300 to 700 ppm. (A.K.)

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

Science.gov (United States)

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

High-performance liquid-chromatographic separation of subcomponents of antimycin-A

Science.gov (United States)

Abidi, S.L.

1988-01-01

Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

Influence of column type and chromatographic conditions on the ion-exchange chromatography of immunoglobulins.

Science.gov (United States)

Yang, Y B; Harrison, K

1996-08-30

Immunoglobulins are often purified by affinity chromatography. However, this technique is costly, can result in poor resolution for subclasses (or is only group specific), and leads to possible leaching of contaminants into the purified products. Ion-exchange chromatography has shown great potential and has found an increased usage in the purification of immunoglobulins. The aim of this study is to further understand the separation mechanism with emphasis on the influence of column type and chromatographic conditions on the peak shape, selectivity and changes in the elution patterns. Included are strong cation-exchange, strong anion-exchange and weak anion-exchange columns. Five immunoglobulin G antibodies were used as test probes. Some sera and ascites were also used in the study. Among the chromatographic conditions examined were mobile phase pH, buffer type, buffer concentration, gradient rate, and column temperature. Significant differences in the chromatographic behavior (elution pattern, peak shape and selectivity) of the test samples are discussed in regard to the column type and the chromatographic conditions.

Chiral ionic liquids in chromatographic and electrophoretic separations.

Science.gov (United States)

Kapnissi-Christodoulou, Constantina P; Stavrou, Ioannis J; Mavroudi, Maria C

2014-10-10

This report provides an overview of the application of chiral ionic liquids (CILs) in separation technology, and particularly in capillary electrophoresis and both gas and liquid chromatography. There is a large number of CILs that have been synthesized and designed as chiral agents. However, only a few have successfully been applied in separation technology. Even though this application of CILs is still in its early stages, the scientific interest is increasing dramatically. This article is focused on the use of CILs as chiral selectors, background electrolyte additives, chiral ligands and chiral stationary phases in electrophoretic and chromatographic techniques. Different examples of CILs, which contain either a chiral cation, a chiral anion or both, are presented in this review article, and their major advantages along with their potential applications in chiral electrophoretic and chromatographic recognition are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Advanced analytical techniques

International Nuclear Information System (INIS)

Mrochek, J.E.; Shumate, S.E.; Genung, R.K.; Bahner, C.T.; Lee, N.E.; Dinsmore, S.R.

1976-01-01

The development of several new analytical techniques for use in clinical diagnosis and biomedical research is reported. These include: high-resolution liquid chromatographic systems for the early detection of pathological molecular constituents in physiologic body fluids; gradient elution chromatography for the analysis of protein-bound carbohydrates in blood serum samples, with emphasis on changes in sera from breast cancer patients; electrophoretic separation techniques coupled with staining of specific proteins in cellular isoenzymes for the monitoring of genetic mutations and abnormal molecular constituents in blood samples; and the development of a centrifugal elution chromatographic technique for the assay of specific proteins and immunoglobulins in human blood serum samples

Principles of qualitative analysis in the chromatographic context.

Science.gov (United States)

Valcárcel, M; Cárdenas, S; Simonet, B M; Carrillo-Carrión, C

2007-07-27

This article presents the state of the art of qualitative analysis in the framework of the chromatographic analysis. After establishing the differences between two main classes of qualitative analysis (analyte identification and sample classification/qualification) the particularities of instrumental qualitative analysis are commented on. Qualitative chromatographic analysis for sample classification/qualification through the so-called chromatographic fingerprint (for complex samples) or the volatiles profile (through the direct coupling headspace-mass spectrometry using the chromatograph as interface) is discussed. Next, more technical exposition of the qualitative chromatographic information is presented supported by a variety of representative examples.

Stereospecific high-performance liquid chromatographic assay of sotalol in plasma.

Science.gov (United States)

Carr, R A; Foster, R T; Bhanji, N H

1991-09-01

A convenient high-performance liquid chromatographic (HPLC) assay was developed for determination of sotalol (STL) enantiomers in plasma. Following addition of the internal standard (IS; racemic atenolol), enantiomers of STL and IS were extracted using ethyl acetate. After evaporation of the organic layer, samples were derivatized with a solution of S-(+)-1-(1-naphthyl)ethyl isocyanate (NEIC). The resulting diastereomers were chromatographed with normal-phase HPLC with chloroform:hexane:methanol [65:33:2 (v/v)] as the mobile phase at a flow rate of 2 ml/min. The fluorescence detection wavelength was set at 220 nm for excitation with no emission filter. The suitability of the assay for pharmacokinetic studies was determined by measuring STL enantiomers in the plasma of a healthy subject after administration of a single 160-mg oral, racemic dose of STL.

Chromatographic separation and spectro-analytical characterization of a natural African mineral dye

Directory of Open Access Journals (Sweden)

G.B. Adebayo

2007-08-01

Full Text Available Chromatographic fractionation and spectroscopic characterization of a natural African mineral dye have been carried out. The chromatographic separation of the dyes made use of column and thin layer chromatographic techniques. Some physicochemical properties of the dye including solubility in polar and non-polar solvents, pH, ash and organic contents were determined. The spectro-analytical techniques used for characterization included energy dispersive X-ray fluorescence (EDXRF, X-ray diffractometry (XRD, Optical microscopy, infrared (IR and UV-VIS spectroscopy. Four different fractions having colours yellow, grey, orange and purple were obtained from the chromatographic separation. All the fractions were found to contain aromatic nucleus based on IR and UV-VIS spectroscopic data. Other functional groups detected are Ar-NH2, -CONH2, C=C, C-C and metal-carbon chelate rings. The presence of aromatic amine in the dye provides strong evidence for its use as hair dye. The dye was found to be soluble in both aqueous and non-aqueous solvents. The pH of the dye's aqueous solution was found to be 8.6, and the ash and organic content of the raw dye were 49 % and 51 % respectively. The XRF revealed that the dye contains twenty elements with concentrations ranging from major to ultra-trace levels. The XRD also showed that the sample contains about forty-six mineral phases which include both inorganic and organic components. The maximum absorption wavelength (λmax in UV-VIS of the aqueous solution was found to be 464 nm. The optical microscopic investigation gave indication that the dyes are likely to be of the marine origin.

Liquid chromatographic separation of terpenoid pigments in foods and food products.

Science.gov (United States)

Cserháti, T; Forgács, E

2001-11-30

The newest achievements in the use of various liquid chromatographic techniques such as adsorption and reversed-phase thin-layer chromatography and HPLC employed for the separation and quantitative determination of terpenoid-based color substances in foods and food products are reviewed. The techniques applied for the analysis of individual pigments and pigments classes are surveyed and critically evaluated. Future trends in the separation and identification of pigments in foods and food products are delineated.

Correlations between chromatographic parameters and bioactivity predictors of potential herbicides.

Science.gov (United States)

Janicka, Małgorzata

2014-08-01

Different liquid chromatography techniques, including reversed-phase liquid chromatography on Purosphere RP-18e, IAM.PC.DD2 and Cosmosil Cholester columns and micellar liqud chromatography with a Purosphere RP-8e column and using buffered sodium dodecyl sulfate-acetonitrile as the mobile phase, were applied to study the lipophilic properties of 15 newly synthesized phenoxyacetic and carbamic acid derivatives, which are potential herbicides. Chromatographic lipophilicity descriptors were used to extrapolate log k parameters (log kw and log km) and log k values. Partitioning lipophilicity descriptors, i.e., log P coefficients in an n-octanol-water system, were computed from the molecular structures of the tested compounds. Bioactivity descriptors, including partition coefficients in a water-plant cuticle system and water-human serum albumin and coefficients for human skin partition and permeation were calculated in silico by ACD/ADME software using the linear solvation energy relationship of Abraham. Principal component analysis was applied to describe similarities between various chromatographic and partitioning lipophilicities. Highly significant, predictive linear relationships were found between chromatographic parameters and bioactivity descriptors. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Gas Chromatographic Determination of Methyl Salicylate in Rubbing Alcohol: An Experiment Employing Standard Addition.

Science.gov (United States)

Van Atta, Robert E.; Van Atta, R. Lewis

1980-01-01

Provides a gas chromatography experiment that exercises the quantitative technique of standard addition to the analysis for a minor component, methyl salicylate, in a commercial product, "wintergreen rubbing alcohol." (CS)

Integrated Analysis of the Wood Oil from Xanthocyparis vietnamensis Farjon & Hiep. by Chromatographic and Spectroscopic Techniques.

Science.gov (United States)

Bazzali, Ophélie; Thai, Tran Huy; Hoi, Tran Minh; Khang, Nguyen Sinh; Hien, Nguyen Thi; Casanova, Joseph; Bighelli, Ange; Tomi, Félix

2016-06-27

In order to get better knowledge about the volatiles produced by Xanthocyparis vietnamensis, a species recently discovered in Vietnam, its wood oil has been analyzed by a combination of chromatographic (GC, CC) and spectroscopic (GC-MS, (13)C-NMR) techniques. Forty components that accounted for 87.9% of the oil composition have been identified. The composition is dominated by nootkatene (20.7%), 11,12,13-tri-nor-eremophil-1(10)-en-7-one (17.2%), γ-eudesmol (5.1%), nootkatone (4.7%), valencene (3.5%) and 13-nor-eremophil-1(10)-en-11-one (2.6%). The structure of two new compounds-10-epi-nor-γ-eudesmen-11-one and 12-hydroxy-isodihydroagarofuran-has been elucidated, while 11,12,13-tri-nor-eremophil-1(10)-en-7-ol is reported as a natural product for the first time. The composition of X. vietnamensis wood oil varied drastically from those of leaf oils, dominated by hedycaryol (34.4%), phyllocladene (37.8%) or by pimara-6(14)-15-diene (19.4%).

Integrated Analysis of the Wood Oil from Xanthocyparis vietnamensis Farjon & Hiep. by Chromatographic and Spectroscopic Techniques

Directory of Open Access Journals (Sweden)

Ophélie Bazzali

2016-06-01

Full Text Available In order to get better knowledge about the volatiles produced by Xanthocyparis vietnamensis, a species recently discovered in Vietnam, its wood oil has been analyzed by a combination of chromatographic (GC, CC and spectroscopic (GC-MS, 13C-NMR techniques. Forty components that accounted for 87.9% of the oil composition have been identified. The composition is dominated by nootkatene (20.7%, 11,12,13-tri-nor-eremophil-1(10-en-7-one (17.2%, γ-eudesmol (5.1%, nootkatone (4.7%, valencene (3.5% and 13-nor-eremophil-1(10-en-11-one (2.6%. The structure of two new compounds—10-epi-nor-γ-eudesmen-11-one and 12-hydroxy-isodihydroagarofuran—has been elucidated, while 11,12,13-tri-nor-eremophil-1(10-en-7-ol is reported as a natural product for the first time. The composition of X. vietnamensis wood oil varied drastically from those of leaf oils, dominated by hedycaryol (34.4%, phyllocladene (37.8% or by pimara-6(14-15-diene (19.4%.

Gas-liquid chromatographic determination of resmethrin in corn, cornmeal, flour, and wheat.

Science.gov (United States)

Simonaitis, R A; Cail, R S

1975-09-01

A gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cis-trans-(+/-)-2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.

Chromatographic and electrophoretic approaches in ink analysis.

Science.gov (United States)

Zlotnick, J A; Smith, F P

1999-10-15

Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

Monitoring for 99Tc in borehole waters using an extraction chromatographic resin

International Nuclear Information System (INIS)

Davis, T.M.; Nelson, D.M.; Thompson, E.G.

1993-01-01

A technique using an extraction chromatographic resin for the analysis of 99 Tc in borehole waters is presented. The method involves one pass of the sample through two resins, a rinse of the resins, then counting of one of the resins by liquid scintillation counting. The technique is intended to be used as a screening method of 99 Tc. The procedure employs commercially available materials, generates little waste and requires very little operator time

Ten years of experience in extraction chromatographic processes for the recovery, separation and purification of actinides elements

International Nuclear Information System (INIS)

Madic, C.; Bourges, J.; Koehly, G.

1984-06-01

Ten years ago the extraction chromatographic technique was developed for preparative purposes and is now applied for all chemicals separations needed for the production of actinides isotopes. That technique appears to be simple and flexible. It can be used for the production of microgram to kilogram amounts of actinide isotopes. This paper focuses on the experience gained and describes some peculiar production of actinide isotopes solved by using extraction chromatographic technique. After a review of extracting molecules and equipment, treatment of irradiated targets (preparation of Pu 238 and removal of neptunium, production of Am 243 and Cm 244), recovery of actinides from alpha aqueous wastes (preparation of Am 241) and recovery of decay products from aged actinide stocks (recovery of Am 241 from Pu stocks, of U 234 from Pu 238 stocks) are described

The co-feature ratio, a novel method for the measurement of chromatographic and signal selectivity in LC-MS-based metabolomics

International Nuclear Information System (INIS)

Elmsjö, Albert; Haglöf, Jakob; Engskog, Mikael K.R.; Nestor, Marika; Arvidsson, Torbjörn; Pettersson, Curt

2017-01-01

Evaluation of analytical procedures, especially in regards to measuring chromatographic and signal selectivity, is highly challenging in untargeted metabolomics. The aim of this study was to suggest a new straightforward approach for a systematic examination of chromatographic and signal selectivity in LC-MS-based metabolomics. By calculating the ratio between each feature and its co-eluting features (the co-features), a measurement of the chromatographic selectivity (i.e. extent of co-elution) as well as the signal selectivity (e.g. amount of adduct formation) of each feature could be acquired, the co-feature ratio. This approach was used to examine possible differences in chromatographic and signal selectivity present in samples exposed to three different sample preparation procedures. The capability of the co-feature ratio was evaluated both in a classical targeted setting using isotope labelled standards as well as without standards in an untargeted setting. For the targeted analysis, several metabolites showed a skewed quantitative signal due to poor chromatographic selectivity and/or poor signal selectivity. Moreover, evaluation of the untargeted approach through multivariate analysis of the co-feature ratios demonstrated the possibility to screen for metabolites displaying poor chromatographic and/or signal selectivity characteristics. We conclude that the co-feature ratio can be a useful tool in the development and evaluation of analytical procedures in LC-MS-based metabolomics investigations. Increased selectivity through proper choice of analytical procedures may decrease the false positive and false negative discovery rate and thereby increase the validity of any metabolomic investigation. - Highlights: • The co-feature ratio (CFR) is introduced. • CFR measures chromatographic and signal selectivity of a feature. • CFR can be used for evaluating experimental procedures in metabolomics. • CFR can aid in locating features with poor selectivity. �

The co-feature ratio, a novel method for the measurement of chromatographic and signal selectivity in LC-MS-based metabolomics

Energy Technology Data Exchange (ETDEWEB)

Elmsjö, Albert, E-mail: Albert.Elmsjo@farmkemi.uu.se [Department of Medicinal Chemistry, Division of Analytical Pharmaceutical Chemistry, Uppsala University (Sweden); Haglöf, Jakob; Engskog, Mikael K.R. [Department of Medicinal Chemistry, Division of Analytical Pharmaceutical Chemistry, Uppsala University (Sweden); Nestor, Marika [Department of Immunology, Genetics and Pathology, Uppsala University (Sweden); Arvidsson, Torbjörn [Department of Medicinal Chemistry, Division of Analytical Pharmaceutical Chemistry, Uppsala University (Sweden); Medical Product Agency, Uppsala (Sweden); Pettersson, Curt [Department of Medicinal Chemistry, Division of Analytical Pharmaceutical Chemistry, Uppsala University (Sweden)

2017-03-01

Evaluation of analytical procedures, especially in regards to measuring chromatographic and signal selectivity, is highly challenging in untargeted metabolomics. The aim of this study was to suggest a new straightforward approach for a systematic examination of chromatographic and signal selectivity in LC-MS-based metabolomics. By calculating the ratio between each feature and its co-eluting features (the co-features), a measurement of the chromatographic selectivity (i.e. extent of co-elution) as well as the signal selectivity (e.g. amount of adduct formation) of each feature could be acquired, the co-feature ratio. This approach was used to examine possible differences in chromatographic and signal selectivity present in samples exposed to three different sample preparation procedures. The capability of the co-feature ratio was evaluated both in a classical targeted setting using isotope labelled standards as well as without standards in an untargeted setting. For the targeted analysis, several metabolites showed a skewed quantitative signal due to poor chromatographic selectivity and/or poor signal selectivity. Moreover, evaluation of the untargeted approach through multivariate analysis of the co-feature ratios demonstrated the possibility to screen for metabolites displaying poor chromatographic and/or signal selectivity characteristics. We conclude that the co-feature ratio can be a useful tool in the development and evaluation of analytical procedures in LC-MS-based metabolomics investigations. Increased selectivity through proper choice of analytical procedures may decrease the false positive and false negative discovery rate and thereby increase the validity of any metabolomic investigation. - Highlights: • The co-feature ratio (CFR) is introduced. • CFR measures chromatographic and signal selectivity of a feature. • CFR can be used for evaluating experimental procedures in metabolomics. • CFR can aid in locating features with poor selectivity. �

Chromatographic hydrogen isotope separation

International Nuclear Information System (INIS)

Aldridge, F.T.

1983-01-01

Intermetallic compounds with the CaCu5 type of crystal structure, particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

Chromatographic hydrogen isotope separation

International Nuclear Information System (INIS)

Aldridge, F.T.

1981-01-01

Intermetallic compounds with the CaCu5 type of crystal structure , particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

New quantitative safety standards: different techniques, different results?

International Nuclear Information System (INIS)

Rouvroye, J.L.; Brombacher, A.C.

1999-01-01

Safety Instrumented Systems (SIS) are used in the process industry to perform safety functions. Many factors can influence the safety of a SIS like system layout, diagnostics, testing and repair. In standards like the German DIN no quantitative analysis is demanded (DIN V 19250 Grundlegende Sicherheitsbetrachtungen fuer MSR-Schutzeinrichtungen, Berlin, 1994; DIN/VDE 0801 Grundsaetze fuer Rechner in Systemen mit Sicherheitsaufgaben, Berlin, 1990). The analysis according to these standards is based on expert opinion and qualitative analysis techniques. New standards like the IEC 61508 (IEC 61508 Functional safety of electrical/electronic/programmable electronic safety-related systems, IEC, Geneve, 1997) and the ISA-S84.01 (ISA-S84.01.1996 Application of Safety Instrumented Systems for the Process Industries, Instrument Society of America, Research Triangle Park, 1996) require quantitative risk analysis but do not prescribe how to perform the analysis. Earlier publications of the authors (Rouvroye et al., Uncertainty in safety, new techniques for the assessment and optimisation of safety in process industry, D W. Pyatt (ed), SERA-Vol. 4, Safety engineering and risk analysis, ASME, New York 1995; Rouvroye et al., A comparison study of qualitative and quantitative analysis techniques for the assessment of safety in industry, P.C. Cacciabue, I.A. Papazoglou (eds), Proceedings PSAM III conference, Crete, Greece, June 1996) have shown that different analysis techniques cover different aspects of system behaviour. This paper shows by means of a case study, that different (quantitative) analysis techniques may lead to different results. The consequence is that the application of the standards to practical systems will not always lead to unambiguous results. The authors therefore propose a technique to overcome this major disadvantage

The combination of the liquid chromatograph with the nuclear magnetic resonance spectrometer

International Nuclear Information System (INIS)

Scott, R.P.W.

1986-01-01

The association of the liquid chromatograph with the NMR spectrometer would be a very powerful analytical system for the separation and identification of unknown mixtures. There are, however, some serious difficulties involved with the association of these two techniques. The historical development of NMR chromatography is outlined and some problems are discussed. (Auth.)

Force coordination in static manipulation tasks performed using standard and non-standard grasping techniques.

Science.gov (United States)

de Freitas, Paulo B; Jaric, Slobodan

2009-04-01

We evaluated coordination of the hand grip force (GF; normal component of the force acting at the hand-object contact area) and load force (LF; the tangential component) in a variety of grasping techniques and two LF directions. Thirteen participants exerted a continuous sinusoidal LF pattern against externally fixed handles applying both standard (i.e., using either the tips of the digits or the palms; the precision and palm grasps, respectively) and non-standard grasping techniques (using wrists and the dorsal finger areas; the wrist and fist grasp). We hypothesized (1) that the non-standard grasping techniques would provide deteriorated indices of force coordination when compared with the standard ones, and (2) that the nervous system would be able to adjust GF to the differences in friction coefficients of various skin areas used for grasping. However, most of the indices of force coordination remained similar across the tested grasping techniques, while the GF adjustments for the differences in friction coefficients (highest in the palm and the lowest in the fist and wrist grasp) provided inconclusive results. As hypothesized, GF relative to the skin friction was lowest in the precision grasp, but highest in the palm grasp. Therefore, we conclude that (1) the elaborate coordination of GF and LF consistently seen across the standard grasping techniques could be generalized to the non-standard ones, while (2) the ability to adjust GF using the same grasping technique to the differences in friction of various objects cannot be fully generalized to the GF adjustment when different grasps (i.e., hand segments) are used to manipulate the same object. Due to the importance of the studied phenomena for understanding both the functional and neural control aspects of manipulation, future studies should extend the current research to the transient and dynamic tasks, as well as to the general role of friction in our mechanical interactions with the environment.

A Small-Scale Low-Cost Gas Chromatograph

Science.gov (United States)

Gros, Natasa; Vrtacnik, Margareta

2005-01-01

The design and application of a small-scale portable gas chromatograph for learning of the basic concepts of chromatography is described. The apparatus consists of two basic separable units, which includes a chromatographic unit and an electronic unit.

Exploring Blueberry Aroma Complexity by Chromatographic and Direct-Injection Spectrometric Techniques.

Science.gov (United States)

Farneti, Brian; Khomenko, Iuliia; Grisenti, Marcella; Ajelli, Matteo; Betta, Emanuela; Algarra, Alberto Alarcon; Cappellin, Luca; Aprea, Eugenio; Gasperi, Flavia; Biasioli, Franco; Giongo, Lara

2017-01-01

, and esters that can be used as putative biomarkers to rapidly evaluate the blueberry aroma variations related to ripening and/or senescence as well as to genetic background differences. Moreover, the obtained results demonstrated the complementarity between chromatographic and direct-injection mass spectrometric techniques to study the blueberry aroma.

Spectroscopic and chromatographic analysis of oil from an oil shale flash pyrolysis unit

Energy Technology Data Exchange (ETDEWEB)

Khraisha, V.H.; Irqsousi, N.A. [University of Jordan, Amman (Jordan). Dept. of Chemical Engineering; Shabib, I.M. [Applied Science Univ., Amman (Jordan). Dept. of Chemistry

2003-01-01

In this investigation, spectroscopic (FT-IR, UV-Vis, {sup 1}H NMR) and chromatographic (GC) techniques were used to analyze two Jordanian shale oils, Sultani and El-Lajjun. The oils were extracted at different pyrolysis temperatures (400-500{sup o}C) using a fluidized bed reactor. The spectroscopic and chromatographic analyses show that the variation of pyrolysis temperature has no significant effect on the composition of the produced oil. The {sup 1}H NMR results indicate that the protons of methyl and methelyene represent the bulk of the hydrogen ({approx}90%) in most shale oil samples. GC analysis reveals that the oil samples contain n-alkanes with a predominant proportion of n-C{sub 25}. (Author)

Chromatographic separation of alkaline phosphatase from dental enamel

DEFF Research Database (Denmark)

Moe, D; Kirkeby, S; Salling, E

1989-01-01

Alkaline phosphatase (AP) was prepared from partly mineralized bovine enamel by extraction in phosphate buffer, centrifugation and various chromatographic techniques. Chromatofocusing showed that the enamel enzyme possessed five isoelectric points at the acid pH level ranging from pH 5.7 to pH 4.......4. Three enzyme peaks were eluted using low pressure chromatography with a Bio-gel column. With a HPLC gel filtration column the separation of the enamel extract resulted in only one peak with AP activity. The fractions of this peak were used to produce an antibody against bovine AP....

Multivariate analysis of chromatographic retention data as a supplementary means for grouping structurally related compounds.

Science.gov (United States)

Fasoula, S; Zisi, Ch; Sampsonidis, I; Virgiliou, Ch; Theodoridis, G; Gika, H; Nikitas, P; Pappa-Louisi, A

2015-03-27

In the present study a series of 45 metabolite standards belonging to four chemically similar metabolite classes (sugars, amino acids, nucleosides and nucleobases, and amines) was subjected to LC analysis on three HILIC columns under 21 different gradient conditions with the aim to explore whether the retention properties of these analytes are determined from the chemical group they belong. Two multivariate techniques, principal component analysis (PCA) and discriminant analysis (DA), were used for statistical evaluation of the chromatographic data and extraction similarities between chemically related compounds. The total variance explained by the first two principal components of PCA was found to be about 98%, whereas both statistical analyses indicated that all analytes are successfully grouped in four clusters of chemical structure based on the retention obtained in four or at least three chromatographic runs, which, however should be performed on two different HILIC columns. Moreover, leave-one-out cross-validation of the above retention data set showed that the chemical group in which an analyte belongs can be 95.6% correctly predicted when the analyte is subjected to LC analysis under the same four or three experimental conditions as the all set of analytes was run beforehand. That, in turn, may assist with disambiguation of analyte identification in complex biological extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic analysis of methadone hydrochloride oral solution.

Science.gov (United States)

Beasley, T H; Ziegler, H W

1977-12-01

A direct and rapid high-performance liquid chromatographic assay for methadone hydrochloride in a flavored oral solution dosage form is described. A syrup sample, one part diluted with three parts of water, is introduced onto a column packed with octadecylsilane bonded on 10 micrometer porous silica gel (reversed phase). A formic acid-ammonium formate-buffered mobile phase is linear programmed with acetonitrile. The absorbance is monitored continuously at 280 or 254 nm, using a flow-through, UV, double-beam photometer. An aqueous methadone hydrochloride solution is used for external standardization. The relative standard deviation was not more than 1.0%. Drug recovery from a syrup base was better than 99.8%.

Determination of hexachlorocyclohexane pesticide residues in wool fat by a combined high-performance liquid chromatographic-gas-liquid chromatographic method

International Nuclear Information System (INIS)

Ali, S.L.

1978-01-01

Beta- and gamma-hexachlorocyclohexane residues were determined in twelve wool fat samples by using a combined high-performance liquid chromatographic (HPLC)-gas-liquid chromatographic (GLC) method. After extraction and chromatographic clean-up on a silca-gel column, the sample was further purified by HPLC on a reversed-phase C-18 column with methanol as the mobile phase. The final determination was effected by GLC with a 1-mCi nickel-63 electron-capture detector. The analytical method was checked by addition of carbon-14-labelled lindane and measurement of the radioactivity in a liquid scintillation counter. (Auth.)

Chromatographic enhancement techniques for the analysis of persistent organic pollutants in environmental samples

Energy Technology Data Exchange (ETDEWEB)

Reiner, E.; Boden, A.; MacPherson, K.; Kolic, T. [Ontario Ministry of the Environment, Ottawa, Ontario (Canada); Dorman, F. [Restek Corporation, Belefonte, PA (United States); Cochran, J. [LECO Corporation, Las Vegas, NV (United States)

2004-09-15

A number of chromatographic enhancements can be made to improve resolution, reduce analysis times and increase peak capacity. Fast GC with TOFMS is able to deconvolute coeluting peaks with unique mass spectra separated by at least 150 ms. Analyte specific columns like Rtx-Dioxin2 can resolve all the 2,3,7,8 containing congeners except 1,2,3,7,8,9-HxCDF. This compound is typically present at the lowest concentration or not detected and makes up less than 1% of the TEQ. Comprehensive 2D GC can be used to separate a number of difficult coelutions for PCBs and other halogenated organics.

Improvement of AC motor reliability from technique standardization

International Nuclear Information System (INIS)

Muniz, P.R.; Faria, M.D.R.; Mendes, M.P.; Silva, J.N.; Dos Santos, J.D.

2005-01-01

The purpose of this paper is to explain the increase of reliability of motors serviced in the Electrical Maintenance Shop of Companhia Siderurgica de Tubarao by standardization of the technique based on Brazilian and International Standards, manufacturer's recommendations and the experience of the maintenance staff. (author)

Improved Chromatographic Bioavailability Estimations

National Research Council Canada - National Science Library

Dorsey, John

1996-01-01

.... Since the inception of reversed phase liquid chromatography there have been many attempts to correlate chromatographic retention with bioavailability and the most often used bulk measure, the octanol...

Exploring Blueberry Aroma Complexity by Chromatographic and Direct-Injection Spectrometric Techniques

Science.gov (United States)

Farneti, Brian; Khomenko, Iuliia; Grisenti, Marcella; Ajelli, Matteo; Betta, Emanuela; Algarra, Alberto Alarcon; Cappellin, Luca; Aprea, Eugenio; Gasperi, Flavia; Biasioli, Franco; Giongo, Lara

2017-01-01

, for the most aldehydes, alcohols, terpenoids, and esters that can be used as putative biomarkers to rapidly evaluate the blueberry aroma variations related to ripening and/or senescence as well as to genetic background differences. Moreover, the obtained results demonstrated the complementarity between chromatographic and direct-injection mass spectrometric techniques to study the blueberry aroma. PMID:28491071

Exploring Blueberry Aroma Complexity by Chromatographic and Direct-Injection Spectrometric Techniques

Directory of Open Access Journals (Sweden)

Brian Farneti

2017-04-01

pull of VOCs, for the most aldehydes, alcohols, terpenoids, and esters that can be used as putative biomarkers to rapidly evaluate the blueberry aroma variations related to ripening and/or senescence as well as to genetic background differences. Moreover, the obtained results demonstrated the complementarity between chromatographic and direct-injection mass spectrometric techniques to study the blueberry aroma.

Chromatographic analysis and purification of multiply tritium-labelled eicosanoids

International Nuclear Information System (INIS)

Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

1988-01-01

A comparative study of different chromatographic techniques (gas-liquid (GLC), thin-layer (TLC), liquid (LC), high-pressure liquid (HPLC) chromatography) is presented. They were applied to the analysis and preparative purification of tritium-labelled eicosanoids with a molar radioactivity of 1.8-8.8 TBq/mmol, obtained by selective hydrogenation and by chemical or enzymic methods. The possibility of analyzing reaction mixtures and isolating individual multiply labelled eicosanoids with a chemical and radiochemical purity of 95-98% was demonstrated. Special features of HPLC for high molar radioactivity eicosanoids are considered. (author) 9 refs.; 6 tabs

Paediatric sutureless circumcision-an alternative to the standard technique.

LENUS (Irish Health Repository)

2012-01-31

INTRODUCTION: Circumcision is one of the most commonly performed surgical procedures in male children. A range of surgical techniques exist for this commonly performed procedure. The aim of this study is to assess the safety, functional outcome and cosmetic appearance of a sutureless circumcision technique. METHODS: Over a 9-year period, 502 consecutive primary sutureless circumcisions were performed by a single surgeon. All 502 cases were entered prospectively into a database including all relevant clinical details and a review was performed. The technique used to perform the sutureless circumcision is a modification of the standard sleeve technique with the use of a bipolar diathermy and the application of 2-octyl cyanoacrylate (2-OCA) to approximate the tissue edges. RESULTS: All boys in this study were pre-pubescent and the ages ranged from 6 months to 12 years (mean age 3.5 years). All patients had this procedure performed as a day case and under general anaesthetic. Complications included: haemorrhage (2.2%), haematoma (1.4%), wound infection (4%), allergic reaction (0.2%) and wound dehiscence (0.8%). Only 9 (1.8%) parents or patients were dissatisfied with the cosmetic appearance. CONCLUSION: The use of 2-OCA as a tissue adhesive for sutureless circumcisions is an alternative to the standard suture technique. The use of this tissue adhesive, 2-OCA, results in comparable complication rates to the standard circumcision technique and results in excellent post-operative cosmetic satisfaction.

Probabilistic peak detection for first-order chromatographic data

NARCIS (Netherlands)

Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

2014-01-01

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by

Development and validation of micellar liquid chromatographic methods for the determination of antibiotics in different matrixes.

Science.gov (United States)

Rambla-Alegre, Maria; Esteve-Romero, Josep; Carda-Broch, Samuel

2011-01-01

Antibiotics are the most important bioactive and chemotherapeutic compounds to be produced by microbiological synthesis, and they have proved their worth in a variety of fields, such as medicinal chemistry, agriculture, and the food industry. Interest in antibiotics has grown in parallel with an increasingly high degree of productivity in the field of analytical applications. Therefore, it is necessary to develop chromatographic procedures capable of determining various drugs simultaneously in the shortest possible time. Micellar liquid chromatography (MLC) is an RP-HPLC technique that offers advantages over conventional HPLC as far as sample preparation, selectivity, and versatility are concerned. Its main advantage is that samples can be injected directly into the chromatographic system with no previous preparation step. This paper mainly focuses on the results of the authors' own recent research and reports the chromatographic conditions for determination of various antibiotics (penicillins, quinolones, and sulfonamides) in different matrixes (pharmaceuticals, biological fluids, and food). The work of other authors on MLC-based antibiotic determination has been included.

Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

Directory of Open Access Journals (Sweden)

Nataša Gros

2013-06-01

Full Text Available This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as completely as possible. The sections—Selected Anions, Selected Cations and Metals—follow. The most essential experimental conditions used in different methods are summarized in tables for a rapid comparison. Techniques encountered in the reviewed articles comprise: direct determinations of ions in untreated samples with ion- or ion-exclusion chromatography, or electrostatic ion chromatography; matrix elimination with column-switching; pre-concentration with a chelation ion chromatography and purge-and-trap pre-concentration. Different detection methods were used: non-suppressed conductometric or suppressed conductometric, direct spectrometric or spectrometric after a post-column derivetization, and inductively coupled plasma in combination with optical emission or mass spectrometry.

Technical artifacts in chromatographic analysis of Tc-99m radiopharmaceuticals

International Nuclear Information System (INIS)

Kowalsky, R.J.; Creekmore, J.R.

1982-01-01

Technical artifacts produced during chromatographic analysis of technetium radiopharmaceuticals were investigated. Such artifacts are, we found, caused by improper spotting and drying techniques; these in turn produce spuriously high impurities in Tc-99m complexes of DTPA, MDP, PPi, and GH. The ITLC-SG/acetone system produces considerable streaking of Tc-complex if the applied spot is large and not dried before development. This results in activity in the solvent front portion of the chromatographic strip indicating falsely high levels of pertechnetate impurity. Proper drying of the applied spot eliminates the artifact. The ITLC-SG/saline system yields falsely high, hydrolyzed-reduced technetium impurities if the spot is allowed to enter the solvent during development. Correct spot placement and size eliminate this problem. Strips that are allowed to dry in room air for several minutes may indicate considerable pertechnetate impurity on the chromatogram; yet this may not actually be present in the radiopharmaceutical vial. Drying spots rapidly with hot air or in a nitrogen atmosphere before development eliminates this problem

Headspace gas chromatographic method for the measurement of difluoroethane in blood.

Science.gov (United States)

Broussard, L A; Broussard, A; Pittman, T; Lafferty, D; Presley, L

2001-01-01

To develop a gas chromatographic assay for the analysis of difluoroethane, a volatile substance, in blood and to determine assay characteristics including linearity, limit of quantitation, precision, and specificity. Referral toxicology laboratory Difluoroethane, a colorless, odorless, highly flammable gas used as a refrigerant blend component and aerosol propellant, may be abused via inhalation. A headspace gas chromatographic procedure for the identification and quantitation of difluoroethane in blood is presented. A methanolic stock standard prepared from pure gaseous difluoroethane was used to prepare whole blood calibrators. Quantitation of difluoroethane was performed using a six-point calibration curve and an internal standard of 1-propanol. The assay is linear from 0 to 115 mg/L including a low calibrator at 4 mg/L, the limit of quantitation. Within-run coefficients of variation at mean concentrations of 13.8 mg/L and 38.5 mg/L were 5.8% and 6.8% respectively. Between-run coefficients of variation at mean concentrations of 15.9 mg/L and 45.7 mg/L were 13.4% and 9.8% respectively. Several volatile substances were tested as potential interfering compounds with propane having a retention time identical to that of difluoroethane. This method requires minimal sample preparation, is rapid and reproducible, can be modified for the quantitation of other volatiles, and could be automated using an automatic sampler/injector system.

Chromatographic fingerprinting: An innovative approach for food 'identitation' and food authentication - A tutorial.

Science.gov (United States)

Cuadros-Rodríguez, Luis; Ruiz-Samblás, Cristina; Valverde-Som, Lucia; Pérez-Castaño, Estefanía; González-Casado, Antonio

2016-02-25

Fingerprinting methods describe a variety of analytical methods that provide analytical signals related to the composition of foodstuffs in a non-selective way such as by collecting a spectrum or a chromatogram. Mathematical processing of the information in such fingerprints may allow the characterisation and/or authentication of foodstuffs. In this context, the particular meaning of 'fingerprinting', in conjunction with 'profiling', is different from the original meanings used in metabolomics. This fact has produced some confusion with the use of these terms in analytical papers. Researchers coming from the metabolomic field could use 'profiling' or 'fingerprinting' on a different way to researchers who are devoted to food science. The arrival of an eclectic discipline, named 'foodomics' has not been enough to allay this terminological problem, since the authors keep on using the terms with both meanings. Thus, a first goal of this tutorial is to clarify the difference between both terms. In addition, the chemical approaches for food authentication, i.e., chemical markers, component profiling and instrumental fingerprinting, have been described. A new term, designated as 'food identitation', has been introduced in order to complete the life cycle of the chemical-based food authentication process. Chromatographic fingerprinting has been explained in detail and some strategies which could be applied has been clarified and discussed. Particularly, the strategies for chromatographic signals acquisition and chromatographic data handling are unified in a single framework. Finally, an overview about the applications of chromatographic (GC and LC) fingerprints in food authentication using different chemometric techniques has been included. Copyright © 2016 Elsevier B.V. All rights reserved.

Probabilistic classification method on multi wavelength chromatographic data for photosynthetic pigments identification

Science.gov (United States)

Prilianti, K. R.; Setiawan, Y.; Indriatmoko, Adhiwibawa, M. A. S.; Limantara, L.; Brotosudarmo, T. H. P.

2014-02-01

Environmental and health problem caused by artificial colorant encourages the increasing usage of natural colorant nowadays. Natural colorant refers to the colorant that is derivate from living organism or minerals. Extensive research topic has been done to exploit these colorant, but recent data shows that only 0.5% of the wide range of plant pigments in the earth has been exhaustively used. Hence development of the pigment characterization technique is an important consideration. High-performance liquid chromatography (HPLC) is a widely used technique to separate pigments in a mixture and identify it. In former HPLC fingerprinting, pigment characterization was based on a single chromatogram from a fixed wavelength (one dimensional) and discard the information contained at other wavelength. Therefore, two dimensional fingerprints have been proposed to use more chromatographic information. Unfortunately this method leads to the data processing problem due to the size of its data matrix. The other common problem in the chromatogram analysis is the subjectivity of the researcher in recognizing the chromatogram pattern. In this research an automated analysis method of the multi wavelength chromatographic data was proposed. Principal component analysis (PCA) was used to compress the data matrix and Maximum Likelihood (ML) classification was applied to identify the chromatogram pattern of the existing pigments in a mixture. Three photosynthetic pigments were selected to show the proposed method. Those pigments are β-carotene, fucoxanthin and zeaxanthin. The result suggests that the method could well inform the existence of the pigments in a particular mixture. A simple computer application was also developed to facilitate real time analysis. Input of the application is multi wavelength chromatographic data matrix and the output is information about the existence of the three pigments.

International Standardization of Library and Documentation Techniques.

Science.gov (United States)

International Federation for Documentation, The Hague (Netherlands).

This comparative study of the national and international standards, rules and regulations on library and documentation techniques adopted in various countries was conducted as a preliminary step in determining the minimal bases for facilitating national and international cooperation between documentalists and librarians. The study compares and…

Implementation of a fully automated process purge-and-trap gas chromatograph at an environmental remediation site

International Nuclear Information System (INIS)

Blair, D.S.; Morrison, D.J.

1997-01-01

The AQUASCAN, a commercially available, fully automated purge-and-trap gas chromatograph from Sentex Systems Inc., was implemented and evaluated as an in-field, automated monitoring system of contaminated groundwater at an active DOE remediation site in Pinellas, FL. Though the AQUASCAN is designed as a stand alone process analytical unit, implementation at this site required additional hardware. The hardware included a sample dilution system and a method for delivering standard solution to the gas chromatograph for automated calibration. As a result of the evaluation the system was determined to be a reliable and accurate instrument. The AQUASCAN reported concentration values for methylene chloride, trichloroethylene, and toluene in the Pinellas ground water were within 20% of reference laboratory values

Liquid chromatographic determination of saccharin in beverages and desserts: complementary collaborative study.

Science.gov (United States)

Sjöberg, A M

1988-01-01

A complementary collaborative study was conducted on a liquid chromatographic method for determination of saccharin in accordance with the latest international recommendations. One industrial and 6 official food control laboratories analyzed 3 samples of a juice, a soft drink, and a dessert at concentration levels of 26-90 mg/L, 33-73 mg/L, and 56-147 mg/kg, respectively. Blind duplicates and a blank were supplied for each type of material at each concentration level. The beverage was chromatographed directly and the dessert was extracted with ethanol before chromatography. Average recoveries were 95-107%. The reproducibility relative standard deviations were 6.4-7.3% for the juice, 9.2-20.6% for the soft drink, and 13.4-16.2% for the dessert. The outlier percentage was 14.3%. The results were compared with those of an earlier collaborative study by Nordic laboratories and with general collaborative results obtained by AOAC.

A review on creatinine measurement techniques.

Science.gov (United States)

Mohabbati-Kalejahi, Elham; Azimirad, Vahid; Bahrami, Manouchehr; Ganbari, Ahmad

2012-08-15

This paper reviews the entire recent global tendency for creatinine measurement. Creatinine biosensors involve complex relationships between biology and micro-mechatronics to which the blood is subjected. Comparison between new and old methods shows that new techniques (e.g. Molecular Imprinted Polymers based algorithms) are better than old methods (e.g. Elisa) in terms of stability and linear range. All methods and their details for serum, plasma, urine and blood samples are surveyed. They are categorized into five main algorithms: optical, electrochemical, impedometrical, Ion Selective Field-Effect Transistor (ISFET) based technique and chromatography. Response time, detection limit, linear range and selectivity of reported sensors are discussed. Potentiometric measurement technique has the lowest response time of 4-10 s and the lowest detection limit of 0.28 nmol L(-1) belongs to chromatographic technique. Comparison between various techniques of measurements indicates that the best selectivity belongs to MIP based and chromatographic techniques. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of chromatographic separation on ASP system interface tension and the countermeasures

Directory of Open Access Journals (Sweden)

Jiawei REN

2016-06-01

Full Text Available Because of the existing chromatographic separation phenomenon, ASP flooding changes original nature of the system. Therefore, in laboratory ultra-low interfacial tension ASP system is preferred for sand packs flow experiment to research on the effect of chromatographic separation on ASP system interface tension. The two parameters of "breakthrough time" and "output difference" are used to describe the degree of chromatographic separation, and the produced fluid interfacial tensions at the outlet end at 120 min is measured. The research shows that there exists chromatographic separation between three chemicals of ASP system, with first polymer breakthrough and finally surfactant breakthrough; there is most serious chromatographic separation between surfactant and polymer, while minimum chromatographic separation between alkali and polymer; chromatographic separation makes ASP interfacial tension increase from 10^-3 magnitude to 10^-2 magnitude, affecting flooding effect of ASP system. Thus, reducing the loss of surfactant in the formation will be the main measure to reduce the degree of chromatographic separation. Using sophorolipid as sacrificial agent to replace part of the surfactant injected into formation before ASP system can effectively reduce the impact of chromatography separation and more effectively improve the ultimate recovery ratio.

Large scale chromatographic separations using continuous displacement chromatography (CDC)

International Nuclear Information System (INIS)

Taniguchi, V.T.; Doty, A.W.; Byers, C.H.

1988-01-01

A process for large scale chromatographic separations using a continuous chromatography technique is described. The process combines the advantages of large scale batch fixed column displacement chromatography with conventional analytical or elution continuous annular chromatography (CAC) to enable large scale displacement chromatography to be performed on a continuous basis (CDC). Such large scale, continuous displacement chromatography separations have not been reported in the literature. The process is demonstrated with the ion exchange separation of a binary lanthanide (Nd/Pr) mixture. The process is, however, applicable to any displacement chromatography separation that can be performed using conventional batch, fixed column chromatography

Gas chromatographic measurement in water-steam circuits

International Nuclear Information System (INIS)

Zschetke, J.; Nieder, R.

1984-01-01

A gas chromatographic technique for measurements in water-steam circuits, which has been well known for many years, has been improved by design modifications. A new type of equipment developed for special measuring tasks on nuclear engineering plant also has a general application. To date measurements have been carried out on the ''Otto Hahn'' nuclear powered ship, on the KNK and AVR experimental nuclear power plants at Karlsruhe and Juelich respectively and on experimental boiler circuits. The measurements at the power plants were carried out under different operating conditions. In addition measurements during the alkali operating mode and during combined cycle operation were carried out on the AVR reactor. It has been possible to draw new conclusion from the many measurements undertaken. (orig.) [de

Evaluation of pesticide adsorption in gas chromatographic injector and column

Directory of Open Access Journals (Sweden)

Gevany Paulino de Pinho

2012-01-01

Full Text Available Components in complex matrices can cause variations in chromatographic response during analysis of pesticides by gas chromatography. These variations are related to the competition between analytes and matrix components for adsorption sites in the chromatographic system. The capacity of the pesticides chlorpyrifos and deltamethrin to be adsorbed in the injector and chromatographic column was evaluated by constructing three isotherms and changing the column heating rate to 10 and 30 ºC min-1. By using ANCOVA to compare the slope of calibration graphs, results showed that the higher the injector temperature (310 ºC the lower the pesticide adsorption. Also, deltamethrin influenced the adsorption of chlorpyrifos on the column chromatographic.

Standardization of Laser Methods and Techniques for Vibration Measurements and Calibrations

International Nuclear Information System (INIS)

Martens, Hans-Juergen von

2010-01-01

The realization and dissemination of the SI units of motion quantities (vibration and shock) have been based on laser interferometer methods specified in international documentary standards. New and refined laser methods and techniques developed by national metrology institutes and by leading manufacturers in the past two decades have been swiftly specified as standard methods for inclusion into in the series ISO 16063 of international documentary standards. A survey of ISO Standards for the calibration of vibration and shock transducers demonstrates the extended ranges and improved accuracy (measurement uncertainty) of laser methods and techniques for vibration and shock measurements and calibrations. The first standard for the calibration of laser vibrometers by laser interferometry or by a reference accelerometer calibrated by laser interferometry (ISO 16063-41) is on the stage of a Draft International Standard (DIS) and may be issued by the end of 2010. The standard methods with refined techniques proved to achieve wider measurement ranges and smaller measurement uncertainties than that specified in the ISO Standards. The applicability of different standardized interferometer methods to vibrations at high frequencies was recently demonstrated up to 347 kHz (acceleration amplitudes up to 350 km/s 2 ). The relative deviations between the amplitude measurement results of the different interferometer methods that were applied simultaneously, differed by less than 1% in all cases.

Generation of gaseous methanol reference standards

International Nuclear Information System (INIS)

Geib, R.C.

1991-01-01

Methanol has been proposed as an automotive fuel component. Reliable, accurate methanol standards are essential to support widespread monitoring programs. The monitoring programs may include quantification of methanol from tailpipe emissions, evaporative emissions, plus ambient air methanol measurements. This paper will present approaches and results in the author's investigation to develop high accuracy methanol standards. The variables upon which the authors will report results are as follows: (1) stability of methanol gas standards, the studies will focus on preparation requirements and stability results from 10 to 1,000 ppmv; (2) cylinder to instrument delivery system components and purge technique, these studies have dealt with materials in contact with the sample stream plus static versus flow injection; (3) optimization of gas chromatographic analytical system will be discussed; (4) gas chromatography and process analyzer results and utility for methanol analysis will be presented; (5) the accuracy of the methanol standards will be qualified using data from multiple studies including: (a) gravimetric preparation; (b) linearity studies; (c) independent standards sources such as low pressure containers and diffusion tubes. The accuracy will be provided as a propagation of error from multiple sources. The methanol target concentrations will be 10 to 500 ppmv

Gas-Chromatographic Determination Of Water In Freon PCA

Science.gov (United States)

Melton, Donald M.

1994-01-01

Gas-chromatographic apparatus measures small concentrations of water in specimens of Freon PCA. Testing by use of apparatus faster and provides greater protection against accidental contamination of specimens by water in testing environment. Automated for unattended operation. Also used to measure water contents of materials, other than Freon PCA. Innovation extended to development of purgeable sampling accessory for gas chromatographs.

Chromatographic methods of the measurements of the chloride compounds in troposphere and stratosphere

International Nuclear Information System (INIS)

Lasa, J.; Rosiek, J.

1992-01-01

The paper contains a description of various chromatographic techniques used for the analysis of the tropospheric techniques used for the analysis of the tropospheric and stratospheric halogenated compounds. The types of the column packings used for separation of halogenated compounds are described. Model chromatograms illustrating the separation of halogenated compounds are presented. The methods of the air sampling and injection for the packed and capillary columns were described. The methods of the preparation of gas calibration mixtures are presented. Operational conditions for electron capture detector used by the authors of quoted paper are also given. (author). 66 refs, 29 figs, 13 tabs

Characterization of crude oils and petroleum products: (I Elution liquid chromatographic separation and gas chromatographic analysis of crude oils and petroleum products

Directory of Open Access Journals (Sweden)

E.O. Odebunmi

2002-12-01

Full Text Available Some physical and chemical properties of samples of light, medium and heavy Nigerian crude oils and petroleum products including gasoline, kerosene and engine oil have been measured and are reported in this paper. The crude oils and petroleum products have also been characterized by fractional distillation and elution liquid chromatography. The fractions obtained from elution liquid chromatography were analyzed using gas chromatography (GC. The GC fractions were identified by comparing the retention time of peaks in the unknown samples with those of components of calibration standard mixtures. The importance of the physico-chemical properties and the significance of the fractional distillation and chromatographic separation methods to industrial process operations have been discussed.

Dynamic Headspace Sampling as an Initial Step for Sample Preparation in Chromatographic Analysis.

Science.gov (United States)

Wojnowski, Wojciech; Majchrzak, Tomasz; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

2017-11-01

This work represents a brief summary of the use of dynamic headspace (DHS) as a technique for sample preparation in chromatographic analysis. Despite numerous developments in the area of analyte isolation and enrichment, DHS remains one of the fundamental methods used with GC. In our opinion, interest in this technique will not diminish significantly because it conforms to stipulations of green analytical chemistry. Moreover, DHS fulfills the need for methods that facilitate detection and determination of analytes present at ultratrace levels in complex matrixes. The main focus of this work was placed on the theoretical fundamentals of this method. Also described herein were DHS development, the advantages and disadvantages of this technique compared with other headspace sampling techniques, and selected examples of its applications in food and environmental analyses.

Estimation of Chromatographic Columns Performances using Computer Tomography and CFD Simulations

DEFF Research Database (Denmark)

Schmidt, Irma; Lottes, Florian; Minceva, Mirjana

2011-01-01

The flow inside a chromatographic column depends decisively on the packed bed inside. Non‐destructive X‐ray computed tomography (CT) was applied as a novel measurement technique to visualize the distribution of velocity and axial dispersion coefficients in preparative scale columns. The results...... show, that spherical particles seem to be more efficient than irregular ones in terms of HETP, which has to be partly a result of the more homogeneous flow profile they induce. The prediction of column performance in dependence of the structure of the packed bed was simulated by CFD (Computational...

Gas-liquid chromatographic determination of aniline metabolites of substituted urea and carbamate herbicides in aqueous solution.

Science.gov (United States)

Hargesheimer, E E; Coutts, R T; Pasutto, F M

1981-07-01

A simple gas-liquid chromatographic (GLC) method has been developed which provides sensitivity and specificity for the analysis of complex mixtures of the commonly occurring herbicide metabolites aniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, and 3-chloro-4-methylaniline. All of these anilines react with acetic anhydride directly in basified aqueous solution. Further reaction of the acetylated anilines with trifluoroacetic anhydride gave diacyl derivatives which were readily resolved by gas chromatography. The structures of the N-acetylated and N-trifluoroacetylated derivatives of benzylamine (internal standard) and the anilines were confirmed by GLC-mass spectrometry. In distilled water the minimum detectable concentrations of aniline and the substituted anilines, using electron capture GLC, are 0.1 nmole/100 mL and 0.05 nmole/100 mL, respectively. The detection limit for the anilines is 1 nmole/100 mL distilled water, using GLC with flame ionization detection. The technique was applied to the determination of anilines added to urine samples obtained from the general population.

Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

International Nuclear Information System (INIS)

Fan Xiaohui; Cheng Yiyu; Ye Zhengliang; Lin Ruichao; Qian Zhongzhi

2006-01-01

Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines

High-performance liquid chromatographic determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine in isoniazid tablet formulations.

Science.gov (United States)

Butterfield, A G; Lovering, E G; Sears, R W

1980-02-01

A high-performance liquid chromatographic procedure is presented for the simultaneous determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine (I) in isoniazid tablet formulations. An aliquot of a diluted aqueous tablet extract is introduced onto a microparticulate cyanopropyl bonded-phase column using a valve-loop injector and chromatographed using a mobile phase of acetonitrile--0.01 M, pH 3.5 aqueous acetate buffer (5:95). Compound I can be determined at levels as low as 0.5% of the isoniazid label claim. The relative standard deviations are 0.4 and 0.7% for the simultaneous determination of isoniazid and I, respectively. Seven commercial tablet formulations contained 93.8--97.0% of the labeled isoniazid amounts and 0.3--5.8% of I, expressed as equivalent isoniazid relative to the labeled isoniazid level.

Miniaturized chromatographic radiochemical procedure for 131I - MIBG

International Nuclear Information System (INIS)

Barboza, M.F. de; Pereira, N.S. de; Colturato, M.T.; Silva, C.P.G. da.

1989-12-01

Different solvents were used in paper chromatographic methods to obtain the best system in routine radiochemical control for 131 I-MIBG produced at IPEN-CNEN/SP. The dates were compared with those obtained with eletrophoresis method in buffer acetate, pH=4.5, 350V, during 40 minutes. The stability of the labeled compound store under 4 0 C was studied during 15 days. Miniaturized chromatographic procedures were established using Whatman 3MM (8x1cm) and n-butanol-:acetic acid: water (S:2:1) as a solvent. the Rf values were: 0.3 (I - ) and 1.0 (MIBG). The radiochemical purity was 99.3 and 99.2% (first day) obtained with eletrophoresis and miniaturized chromatographic procedures, respectively and, 84.7% after 15 days of its preparation. It is a rapid, practical and reproductive method. (author) [pt

Chromatographic separation of Iodine species for environmental studies

Energy Technology Data Exchange (ETDEWEB)

Machado, E.C. [Universidade Federal Fluminense, Niteroi, RJ (Brazil). Dept. de Geoquimica]. E-mail: geoedin@vm.uff.br; Bellido, A.V.B. [Universidade Federal Fluminense, Niteroi, RJ (Brazil). Dept. de Fisico-Quimica]. E-mail: alf@risc2.rmn.uff.br; Bellido, L.F. [Comissao Nacional de Energia Nuclear (CNEN), Rio de Janeiro, RJ (Brazil)]. E-mail: lbellido@cnen.gov.br

1999-07-01

In this work a experimental method was developed to separate iodine species from environmental samples by using adsorption chromatography. The radionuclide {sup 123} I which has a half-life of 13 h and a convenient gamma ray of 159 keV was used to investigate a fast and efficient procedure for the separation of iodide and iodate ions in seawater from mangrove samples. The radio-iodine tracer technique is very useful, particularly in kinetic studies because it is easy to detect without any interference of concentration due to the small amount of tracer that is spiked. It is also possible to add two tracers (I-123 and I-131) in different oxidation states. Three chromatographic methods were studied: paper, thin layer and adsorption chromatography with silica and alumina. It was found that paper chromatography is very useful for checking the valence adjustment of the radioiodine species. Initially, several coefficient distributions of iodine species by adsorption in silica and alumina from NaOH, NaHCO{sub 3} and NaNO{sub 3} solutions (in the range 05. - 0.0001 m) were determined. The best separation so far was achieved by loading the sample (after adjusting the concentration to 0.1 NNaNO{sub 3}) into a chromatographic column with Al{sub 2} O{sub 3}. The iodide passes through the column and after washing the column, the iodate was removed by eluting with 1.0 M NaHCO{sub 3} solution. (author)

Chromatographic separation of Iodine species for environmental studies

International Nuclear Information System (INIS)

Machado, E.C.

1999-01-01

In this work a experimental method was developed to separate iodine species from environmental samples by using adsorption chromatography. The radionuclide 123 I which has a half-life of 13 h and a convenient gamma ray of 159 keV was used to investigate a fast and efficient procedure for the separation of iodide and iodate ions in seawater from mangrove samples. The radio-iodine tracer technique is very useful, particularly in kinetic studies because it is easy to detect without any interference of concentration due to the small amount of tracer that is spiked. It is also possible to add two tracers (I-123 and I-131) in different oxidation states. Three chromatographic methods were studied: paper, thin layer and adsorption chromatography with silica and alumina. It was found that paper chromatography is very useful for checking the valence adjustment of the radioiodine species. Initially, several coefficient distributions of iodine species by adsorption in silica and alumina from NaOH, NaHCO 3 and NaNO 3 solutions (in the range 05. - 0.0001 m) were determined. The best separation so far was achieved by loading the sample (after adjusting the concentration to 0.1 NNaNO 3 ) into a chromatographic column with Al 2 O 3 . The iodide passes through the column and after washing the column, the iodate was removed by eluting with 1.0 M NaHCO 3 solution. (author)

Standard lymphadenectomy technique in the gastric adenocarcinoma

International Nuclear Information System (INIS)

Aguirre Fernandez, Roberto Eduardo; Fernandez Vazquez, Pedro Ivan; LLera Dominguez, Gerardo de la

2012-01-01

The surgical technique used from 1990 in the 'Celia Sanchez Manduley' Clinical Surgical Teaching Provincial Hospital in Manzanillo, Granma province to carry out the gastrectomy together with the standard lymphadenectomy in patients carriers of a gastric adenocarcinoma, allowing application of the current oncologic and surgical concepts of the Japanese Society for Research of Gastric Cancer, essential to obtain a better prognosis in these patients

[Study on standardization of cupping technique: elucidation on the establishment of the National Standard Standardized Manipulation of Acupuncture and Moxibustion, Part V, Cupping].

Science.gov (United States)

Gao, Shu-zhong; Liu, Bing

2010-02-01

From the aspects of basis, technique descriptions, core contents, problems and solutions, and standard thinking in standard setting process, this paper states experiences in the establishment of the national standard Standardized Manipulation of Acupuncture and Moxibustion, Part V, Cupping, focusing on methodologies used in cupping standard setting process, the method selection and operating instructions of cupping standardization, and the characteristics of standard TCM. In addition, this paper states the scope of application, and precautions for this cupping standardization. This paper also explaines tentative ideas on the research of standardized manipulation of acupuncture and moxibustion.

Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

Energy Technology Data Exchange (ETDEWEB)

Fan Xiaohui [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China); Cheng Yiyu [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China)]. E-mail: chengyy@zju.edu.cn; Ye Zhengliang [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China); Lin Ruichao [National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050 (China); Qian Zhongzhi [Committee of Chinese Pharmacopoeia, Beijing 100061 (China)

2006-01-12

Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines.

Determination of the analytical performance of a headspace capillary gas chromatographic technique and karl Fischer coulometric titration by system calibration using oil samples containing known amounts of moisture.

Science.gov (United States)

Jalbert, J; Gilbert, R; Tétreault, P

1999-08-01

Over the past few years, concerns have been raised in the literature about the accuracy of the Karl Fischer (KF) method for assessing moisture in transformer mineral oils. To better understand this issue, the performance of a static headspace capillary gas chromatographic (HS-CGC) technique was compared to that of KF coulometric titration by analyzing moisture in samples containing known amounts of water and various samples obtained from the National Institute of Standards and Technology (NIST). Two modes of adding samples into the KF vessel were used:  direct injection and indirect injection via an azeotropic distillation of the moisture with toluene. Under the conditions used for direct injection, the oil matrix was totally dissolved in the anolyte, which allowed the moisture to be titrated in a single-phase solution rather than in a suspension. The results have shown that when HS-CGC and combined azeotropic distillation/KF titration are calibrated with moisture-in-oil standards, a linear relation is observed over 0-60 ppm H(2)O with a correlation coefficient better than 0.9994 (95% confidence), with the regression line crossing through zero. A similar relation can also be observed when calibration is achieved by direct KF addition of standards prepared with octanol-1, but in this case an intercept of 4-5 ppm is noted. The amount of moisture determined by curve interpolation in NIST reference materials by the three calibrated systems ranges from 13.0 to 14.8 ppm for RM 8506 and 42.5 to 46.4 ppm for RM 8507, and in any case, the results were as high as those reported in the literature with volumetric KF titration. However, titration of various dehydrated oil and solvent samples showed that direct KF titration is affected by a small bias when samples contain very little moisture. The source of error after correction for the large sample volume used for the determination (8 mL) is about 6 ppm for Voltesso naphthenic oil and 4 ppm for toluene, revealing a matrix

A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

Energy Technology Data Exchange (ETDEWEB)

Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

2004-09-15

Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

Direct chromatographic methods for the rapid determination of homogentisic acid in strawberry tree (Arbutus unedo L.) honey.

Science.gov (United States)

Scanu, Roberta; Spano, Nadia; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Sanna, Gavino; Tapparo, Andrea

2005-10-07

Two rapid and direct chromatographic methods based on reverse phase-high performance liquid chromatography (RP-HPLC) and ion chromatography (IC) were developed for the determination of homogentisic acid (HA) in honey. This is the marker of the botanic origin of strawberry tree honey. The methods were validated and tested using 22 samples from Sardinia, Italy. The IC method is faster than the RP-HPLC one (6 min versus 13 min of total run), but it is slightly less sensitive (the limit of detection (LOD), is 26 mg kg(-1) versus 15 mg kg(-1)) and reproducible (relative standard deviation, RSD, of 10.4 and 4.4%, respectively). The whole dataset of validation parameters allows both the proposed methods to be considered as bias-free (by recovery tests, comparison of analytical results of the two independent methods and analysis of a synthetic sample) and precise (both the techniques show a repeatability better than 2% repeatability in the range between 70 and 600 mg kg(-1)).

Chromatographical Analysis of Amino Acids in Sepia Mutant of Drosophila melanogaster under Stress of Cypermethrin and Alphamethrin

Directory of Open Access Journals (Sweden)

Namrata Rana

2014-07-01

Full Text Available Insects are invertebrates that are taxonomically referred to as the class Insecta. They are the most numerous and most widespread terrestrial taxon within the phylum Arthropoda, and indeed the most diverse group of animals on the earth, with around 925,000 species described—more than all other animal groups combined. Insects may be found in nearly all environments on the planet, although only a small number of species have adapted to life in the oceans where crustaceans tend to predominate instead. HPTLC is a method commonly applied for the identification, assay and the testing for purity, stability, dissolution or content uniformity of raw materials (herbal and animal extracts, fermentation mixtures, drugs and excipients and formulated products (pharmaceuticals, cosmetics, nutrients. These flexible and cost-effective techniques present the advantage of the simultaneous processing of standards and samples with versatile detection possibilities, including a great variety of post-chromatographic derivatization reagents.

Technique for fabrication of gradual standards of radiographic image blachening density

International Nuclear Information System (INIS)

Borovin, I.V.; Kondina, M.A.

1987-01-01

The technique of fabrication of gradual standards of blackening density for industrial radiography by contact printing from a negative is described. The technique is designed for possibilities of industrial laboratoriesof radiation defectoscopy possessing no special-purpose sensitometric equipment

Standard Establishment Through Scenarios (SETS): A new technique for occupational fitness standards.

Science.gov (United States)

Blacklock, R E; Reilly, T J; Spivock, M; Newton, P S; Olinek, S M

2015-01-01

An objective and scientific task analysis provides the basis for establishing legally defensible Physical Employment Standards (PES), based on common and essential occupational tasks. Infrequent performance of these tasks creates challenges when developing PES based on criterion, or content validity. Develop a systematic approach using Subject Matter Experts (SME) to provide tasks with 1) an occupationally relevant scenario considered common to all personnel; 2) a minimum performance standard defined by time, distance, load or work. Examples provided here relate to the development of a new PES for the Canadian Armed Forces (CAF). SME of various experience are selected based on their eligibility criteria. SME are required to define a reasonable scenario for each task from personal experience, provide occupational performance requirements of the scenario in sub-groups, and discuss and agree by consensus vote on the final standard based on the definition of essential. A common and essential task for the CAF is detailed as a case example of process application. Techniques to avoid common SME rating errors are discussed and advantages to the method described. The SETS method was developed as a systematic approach to setting occupational performance standards and qualifying information from SME.

Analyzing chromatographic data using multilevel modeling.

Science.gov (United States)

Wiczling, Paweł

2018-06-01

It is relatively easy to collect chromatographic measurements for a large number of analytes, especially with gradient chromatographic methods coupled with mass spectrometry detection. Such data often have a hierarchical or clustered structure. For example, analytes with similar hydrophobicity and dissociation constant tend to be more alike in their retention than a randomly chosen set of analytes. Multilevel models recognize the existence of such data structures by assigning a model for each parameter, with its parameters also estimated from data. In this work, a multilevel model is proposed to describe retention time data obtained from a series of wide linear organic modifier gradients of different gradient duration and different mobile phase pH for a large set of acids and bases. The multilevel model consists of (1) the same deterministic equation describing the relationship between retention time and analyte-specific and instrument-specific parameters, (2) covariance relationships relating various physicochemical properties of the analyte to chromatographically specific parameters through quantitative structure-retention relationship based equations, and (3) stochastic components of intra-analyte and interanalyte variability. The model was implemented in Stan, which provides full Bayesian inference for continuous-variable models through Markov chain Monte Carlo methods. Graphical abstract Relationships between log k and MeOH content for acidic, basic, and neutral compounds with different log P. CI credible interval, PSA polar surface area.

Chromatographic quality control procedures for /sup 99m/Tc-diagnostic agents

International Nuclear Information System (INIS)

Marinelli, M.; Pozzato, R.; Garuti, P.; Zucchini, G.L.

1986-01-01

The purpose of this work was to experiment simple and rapid chromatographic systems, based on paper and thin-layer techniques, to test the radiochemical purity of some common /sup 99m/Tc diagnostic agents, and select those systems able to prevent the anomalies due to oxidation and artifact production. The agents were examined under conditions which usually bring about the above mentioned anomalies, then the results were compared with those obtained under controlled conditions. Quali- and quantitative detection of the activity present on the chromatograms was carried out using the equipment available in nuclear medicine departments

Approaches to characterise chromatographic column performance based on global parameters accounting for peak broadening and skewness.

Science.gov (United States)

Baeza-Baeza, J J; Pous-Torres, S; Torres-Lapasió, J R; García-Alvarez-Coque, M C

2010-04-02

Peak broadening and skewness are fundamental parameters in chromatography, since they affect the resolution capability of a chromatographic column. A common practice to characterise chromatographic columns is to estimate the efficiency and asymmetry factor for the peaks of one or more solutes eluted at selected experimental conditions. This has the drawback that the extra-column contributions to the peak variance and skewness make the peak shape parameters depend on the retention time. We propose and discuss here the use of several approaches that allow the estimation of global parameters (non-dependent on the retention time) to describe the column performance. The global parameters arise from different linear relationships that can be established between the peak variance, standard deviation, or half-widths with the retention time. Some of them describe exclusively the column contribution to the peak broadening, whereas others consider the extra-column effects also. The estimation of peak skewness was also possible for the approaches based on the half-widths. The proposed approaches were applied to the characterisation of different columns (Spherisorb, Zorbax SB, Zorbax Eclipse, Kromasil, Chromolith, X-Terra and Inertsil), using the chromatographic data obtained for several diuretics and basic drugs (beta-blockers). Copyright (c) 2010 Elsevier B.V. All rights reserved.

Use of the Keele injector for sample introduction for gas chromatographic analysis of vinclozolin in lettuces.

Science.gov (United States)

Shim, J H; Lee, Y S; Kim, M R; Lee, C J; Kim, I S

2003-10-10

We examined a Keele injector for sample introduction for gas chromatographic analysis of vinclozolin treated in lettuces. Samples in milligram quantity were introduced into a glass tube in a Keele injector at a gas chromatograph injection port. The glass tube was then crushed to allow the sample to carry onto a capillary column in a normal manner. The standard calibration curve for quantitative detection of vinclozolin was obtained by determining vinclozolin spiked in samples at variable concentrations. The calibration curve showed a linear response to vinclozolin ranging from 0.05 to 1.0 microg/g, giving a slope value of 174.8, the y-intercept value of -2.8146 and the mean r2-value of 0.9994. Limit of quantification for vinclozolin was 0.05 microg/g by this method, comparable to 0.01 microg/g by a normal injector. When samples treated previously with vinclozolin were determined by the Keele injector, vinclozolin was found to be about 30% lower as compared to a normal method, suggesting about 70% recovery of the spiked vinclozolin by the Keele injector. From these results, the Keele injector was suggested to be potential for sample introduction in gas chromatographic analysis of vinclozolin in lettuce samples.

Mixed-mode chromatographic matrices for the resolution of transfer ribonucleic acids

NARCIS (Netherlands)

Bischoff, Rainer; Mclaughlin, L.W.

1984-01-01

Modification of approximately 65% of the amine groups of an aminopropylsilyl bonded-phase silica high-performance liquid chromatographic anion exchanger (APS-Hypersil) with organic acids containing n-alkyl moieties of different chain lengths, results in mixed mode chromatographic matrices of varying

Performance of chromatographic systems to model soil-water sorption.

Science.gov (United States)

Hidalgo-Rodríguez, Marta; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

2012-08-24

A systematic approach for evaluating the goodness of chromatographic systems to model the sorption of neutral organic compounds by soil from water is presented in this work. It is based on the examination of the three sources of error that determine the overall variance obtained when soil-water partition coefficients are correlated against chromatographic retention factors: the variance of the soil-water sorption data, the variance of the chromatographic data, and the variance attributed to the dissimilarity between the two systems. These contributions of variance are easily predicted through the characterization of the systems by the solvation parameter model. According to this method, several chromatographic systems besides the reference octanol-water partition system have been selected to test their performance in the emulation of soil-water sorption. The results from the experimental correlations agree with the predicted variances. The high-performance liquid chromatography system based on an immobilized artificial membrane and the micellar electrokinetic chromatography systems of sodium dodecylsulfate and sodium taurocholate provide the most precise correlation models. They have shown to predict well soil-water sorption coefficients of several tested herbicides. Octanol-water partitions and high-performance liquid chromatography measurements using C18 columns are less suited for the estimation of soil-water partition coefficients. Copyright © 2012 Elsevier B.V. All rights reserved.

Chromatographic and biological aspects of organomercurials

Energy Technology Data Exchange (ETDEWEB)

Fishbein, L

1970-01-01

A thorough review on the biological and chromatographic aspects of methylmercury, phenylmercurials, and miscellaneous organomercurials is presented. Areas covered include ecology, epidemiology, paper chromatography, thin-layer chromatography, gas chromatography, metabolism and toxicity, and environmental degradation. 183 references.

Chromatographic methods

International Nuclear Information System (INIS)

Marhol, M.; Stary, J.

1975-01-01

The characteristics are given of chromatographic separation and the methods are listed. Methods and data on materials used in partition, adsorption, precipitation and ion exchange chromatography are listed and conditions are described under which ion partition takes place. Special attention is devoted to ion exchange chromatography where tables are given to show the course of values of the partition coefficients of different ions in dependence on the concentration of agents and the course of equilibrium sorptions on different materials in dependence on the solution pH. A theoretical analysis is given and the properties of the most widely used ion exchangers are listed. Experimental conditions and apparatus used for each type of chromatography are listed. (L.K.)

Resolving and quantifying overlapped chromatographic bands by transmutation

Science.gov (United States)

Malinowski

2000-09-15

A new chemometric technique called "transmutation" is developed for the purpose of sharpening overlapped chromatographic bands in order to quantify the components. The "transmutation function" is created from the chromatogram of the pure component of interest, obtained from the same instrument, operating under the same experimental conditions used to record the unresolved chromatogram of the sample mixture. The method is used to quantify mixtures containing toluene, ethylbenzene, m-xylene, naphthalene, and biphenyl from unresolved chromatograms previously reported. The results are compared to those obtained using window factor analysis, rank annihilation factor analysis, and matrix regression analysis. Unlike the latter methods, the transmutation method is not restricted to two-dimensional arrays of data, such as those obtained from HPLC/DAD, but is also applicable to chromatograms obtained from single detector experiments. Limitations of the method are discussed.

A Quantitative Gas Chromatographic Ethanol Determination.

Science.gov (United States)

Leary, James J.

1983-01-01

Describes a gas chromatographic experiment for the quantitative determination of volume percent ethanol in water ethanol solutions. Background information, procedures, and typical results are included. Accuracy and precision of results are both on the order of two percent. (JN)

Chromatographic separation of rhenium in alumina-methanol/sulfuric acid system

International Nuclear Information System (INIS)

Oguma, Koichi

1983-01-01

The adsorption behavior of a number of metals on alumina was surveyed in a methanol-(0.005 -- 0.5) M H 2 SO 4 (3 : 1 v/v) developing solvent by thin-layer chromatography. Over the acid concentration range tested, Re(VII) does not favor the alumina phase to any great extent while the most other metals are strongly adsorbed on alumina. These findings allowed to establish a column chromatographic technique for selective separation of rhenium in a methanol-0.05 M H 2 SO 4 (3 : 1 v/v) eluent. The separation technique thus established was applied to molybdenite analysis for rhenium. About 100-mg powdered sample containing ca. 100 ppm rhenium was decomposed with HNO 3 and then evaporated nearly to dryness. The residue was dissolved in NH 4 OH and the excess NH 4 OH was expelled by evaporation to dryness. The residue was dissolved in 2.5-ml 0.5 M H 2 SO 4 and 10-ml water, the insoluble materials filtered off, and the filtrate diluted to exactly 25 ml with water. A 10-ml aliquot of this solution was mixed with 30-ml methanol and the mixture was passed through a column (diameter 15 mm, bed height 30 mm) containing 5 g of alumina. The column was then washed with 20 ml of a methanol-0.05 M H 2 SO 4 (3 : 1 v/v) mixture. Rhenium was recovered from the loaded solution and the subsequent washings, and was determined spectrophotometrically with Methylene Blue as a chromogenic reagent. The values obtained from four samples of molybdenite are in good agreement with those obtained by neutron activation analysis. The relative standard deviation (n = 4; calculated from the range) was between 2.0 and 5.2 %. (author)

Standardization of surgical techniques used in facial bone contouring.

Science.gov (United States)

Lee, Tae Sung

2015-12-01

Since the introduction of facial bone contouring surgery for cosmetic purposes, various surgical methods have been used to improve the aesthetics of facial contours. In general, by standardizing the surgical techniques, it is possible to decrease complication rates and achieve more predictable surgical outcomes, thereby increasing patient satisfaction. The technical strategies used by the author to standardize facial bone contouring procedures are introduced here. The author uses various pre-manufactured surgical tools and hardware for facial bone contouring. During a reduction malarplasty or genioplasty procedure, double-bladed reciprocating saws and pre-bent titanium plates customized for the zygomatic body, arch and chin are used. Various guarded oscillating saws are used for mandibular angloplasty. The use of double-bladed saws and pre-bent plates to perform reduction malarplasty reduces the chances of post-operative asymmetry or under- or overcorrection of the zygoma contours due to technical faults. Inferior alveolar nerve injury and post-operative jawline asymmetry or irregularity can be reduced by using a guarded saw during mandibular angloplasty. For genioplasty, final placement of the chin in accordance with preoperative quantitative analysis can be easily performed with pre-bent plates, and a double-bladed saw allows more procedural accuracy during osteotomies. Efforts by the surgeon to avoid unintentional faults are key to achieving satisfactory results and reducing the incidence of complications. The surgical techniques described in this study in conjunction with various in-house surgical tools and modified hardware can be used to standardize techniques to achieve aesthetically gratifying outcomes. Copyright © 2015 British Association of Plastic, Reconstructive and Aesthetic Surgeons. Published by Elsevier Ltd. All rights reserved.

Liquid chromatographic analysis of phenobarbitone, ethosuximide ...

African Journals Online (AJOL)

A liquid chromatographic method for the simultaneous assay of four anticonvulsant drugs, phenobarbitone, ethosuximide, phenytoin and carbamazepine on a polystyrene-divinyl benzene column is described. The method was developed by the systematic study of different types of co-polymer materials, type and ...

Rapid planar chromatographic analysis of 25 water-soluble dyes used as food additives.

Science.gov (United States)

Morlock, Gertrud E; Oellig, Claudia

2009-01-01

A rapid planar chromatographic method for identification and quantification of 25 water-soluble dyes in food was developed. In a horizontal developing chamber, the chromatographic separation on silica gel 60F254 high-performance thin-layer chromatography plates took 12 min for 40 runs in parallel, using 8 mL ethyl acetate-methanol-water-acetic acid (65 + 23 + 11 + 1, v/v/v/v) mobile phase up to a migration distance of 50 mm. However, the total analysis time, inclusive of application and evaluation, took 60 min for 40 runs. Thus, the overall time/run can be calculated as 1.5 min with a solvent consumption of 200 microL. A sample throughput of 1000 runs/8 h day can be reached by switching between the working stations (application, development, and evaluation) in a 20 min interval, which triples the analysis throughput. Densitometry was performed by absorption measurement using the multiwavelength scan mode in the UV and visible ranges. Repeatabilities [relative standard deviation (RSD), 4 determinations] at the first or second calibration level showed precisions of mostly or = 0.9987) and RSD values ( or = 0.9996). If necessary for confirmation, online mass spectra were recorded within a minute.

Gas chromatographic sensing on an optical fiber by mode-filtered light detection.

Science.gov (United States)

Bruckner, C A; Synovec, R E

1996-06-01

A chemical sensor for gas phase measurements is reported which combines the principles of chemical separation and fiber optic detection. The analyzer incorporates an annular column Chromatographic sensor, constructed by inserting a polymer-clad optical fiber into a silica capillary. Light from a helium-neon laser is launched down the fiber, producing a steady intensity distribution within the fiber, but a low background of scattered light. When sample vapor is introduced to the sensor, and an analyte-rich volume interacts with the polymer cladding, Chromatographic retention is observed simultaneously with a change in the local refractive index of the cladding. An increase in cladding refractive index (RI) causes light to be coupled out of the fiber, with detection at a right-angle to the annular column length to provide optimum S/N ratio. This detection mechanism is called mode-filtered light detection. We report a gas Chromatographic separation on a 3.1 m annular column (320 microm i.d. silica tube, 228 microm o.d. fiber with a 12 microm fluorinated silicone clad) of methane, benzene, butanone and chlorobenzene in 6 min. The annular column length was reduced to 22 cm to function as a sensor, with selected organic vapors exhibiting unique retention times and detection selectivity. The detection selectivity is determined by the analyte RI and the partition coefficient into the cladding. The calculated limit of detection (LOD) for benzene vapor is 0.03% by volume in nitrogen, and several chlorinated species had LOD values less than 1%. For binary mixtures of organic vapors, the detected response appears to be the linear combination of the two organic standards, suggesting that the annular column may be useful as a general approach for designing chemical sensors that incorporate separation and optical detection principles simultaneously.

An integrated methodological approach to the computer-assisted gas chromatographic screening of basic drugs in biological fluids using nitrogen selective detection.

Science.gov (United States)

Dugal, R; Massé, R; Sanchez, G; Bertrand, M J

1980-01-01

This paper presents the methodological aspects of a computerized system for the gas-chromatographic screening and primary identification of central nervous system stimulants and narcotic analgesics (including some of their respective metabolites) extracted from urine. The operating conditions of a selective nitrogen detector for optimized analytical functions are discussed, particularly the effect of carrier and fuel gas on the detector's sensitivity to nitrogen-containing molecules and discriminating performance toward biological matrix interferences. Application of simple extraction techniques, combined with rapid derivatization procedures, computer data acquisition, and reduction of chromatographic data are presented. Results show that this system approach allows for the screening of several drugs and their metabolites in a short amount of time. The reliability and stability of the system have been tested by analyzing several thousand samples for doping control at major international sporting events and for monitoring drug intake in addicts participating in a rehabilitation program. Results indicate that these techniques can be used and adapted to many different analytical toxicology situations.

ELISA technique standardization for strongyloidiasis diagnosis

International Nuclear Information System (INIS)

Huapaya, P.; Espinoza, I.; Huiza, A.; Universidad Nacional Mayor de San Marcos, Lima; Sevilla, C.

2002-01-01

To standardize ELISA technique for human Strongyloides stercoralis infection diagnosis a crude antigen was prepared using filariform larvae obtained from positive stool samples cultured with charcoal. Harvested larvae were crushed by sonication and washed by centrifugation in order to obtain protein extracts to be used as antigen. Final protein concentration was 600 μg/mL. Several kinds of ELISA plates were tested and antigen concentration, sera dilution, conjugate dilution and cut off were determined to identify infection. Sera from patients with both hyper-infection syndrome and intestinal infection demonstrated by parasitological examination were positive controls and sera from people living in non-endemic areas with no infection demonstrated by parasitological examination were negative controls. Best values were 5 μg/mL for antigen, 1/64 for sera, 1/1000 for conjugate; optical density values for positive samples were 1,2746 (1,1065 - 1,4206, DS = 0,3284) and for negative samples 0,4457 (0,3324 - 0,5538, DS = 0,2230). Twenty sera samples from positive subjects and one hundred from negative subjects were examined, obtaining 90% sensitivity and 88% specificity. The results show this technique could be useful as strongyloidiasis screening test in population studies

Data compression techniques and the ACR-NEMA digital interface communications standard

International Nuclear Information System (INIS)

Zielonka, J.S.; Blume, H.; Hill, D.; Horil, S.C.; Lodwick, G.S.; Moore, J.; Murphy, L.L.; Wake, R.; Wallace, G.

1987-01-01

Data compression offers the possibility of achieving high, effective information transfer rates between devices and of efficient utilization of digital storge devices in meeting department-wide archiving needs. Accordingly, the ARC-NEMA Digital Imaging and Communications Standards Committee established a Working Group to develop a means to incorporate the optimal use of a wide variety of current compression techniques while remaining compatible with the standard. This proposed method allows the use of public domain techniques, predetermined methods between devices already aware of the selected algorithm, and the ability for the originating device to specify algorithms and parameters prior to transmitting compressed data. Because of the latter capability, the technique has the potential for supporting many compression algorithms not yet developed or in common use. Both lossless and lossy methods can be implemented. In addition to description of the overall structure of this proposal, several examples using current compression algorithms are given

Mars Solar Balloon Landed Gas Chromatograph Mass Spectrometer

Science.gov (United States)

Mahaffy, P.; Harpold, D.; Niemann, H.; Atreya, S.; Gorevan, S.; Israel, G.; Bertaux, J. L.; Jones, J.; Owen, T.; Raulin, F.

1999-01-01

A Mars surface lander Gas Chromatograph Mass Spectrometer (GCMS) is described to measure the chemical composition of abundant and trace volatile species and isotope ratios for noble gases and other elements. These measurements are relevant to the study of atmospheric evolution and past climatic conditions. A Micromission plan is under study where a surface package including a miniaturized GCMS would be delivered to the surface by a solar heated hot air balloon based system. The balloon system would be deployed about 8 km above the surface of Mars, wherein it would rapidly fill with Martian atmosphere and be heated quickly by the sun. The combined buoyancy and parachuting effects of the solar balloon result in a surface package impact of about 5 m/sec. After delivery of the package to the surface, the balloon would ascend to about 4 km altitude, with imaging and magnetometry data being taken for the remainder of the daylight hours as the balloon is blown with the Martian winds. Total atmospheric entry mass of this mission is estimated to be approximately 50 kg, and it can fit as an Ariane 5 piggyback payload. The GCMS would obtain samples directly from the atmosphere at the surface and also from gases evolved from solid phase material collected from well below the surface with a Sample Acquisition and Transport Mechanism (SATM). The experiment envisioned in the Mars Micromission described would obtain samples from a much greater depth of up to one meter below the surface, and would search for organic molecules trapped in ancient stratified layers well below the oxidized surface. Insitu instruments on upcoming NASA missions working in concert with remote sensing measurement techniques have the potential to provide a more detailed investigation of mineralogy and the extent of simple volatiles such as CO2 and H2O in surface and subsurface solid phase materials. Within the context of subsequent mission opportunities such as those provided by the Ariane 5 piggyback

On-line gas chromatographic analysis of airborne particles

Science.gov (United States)

Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

2012-01-03

A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

Standardization of proton-induced x-ray emission technique for analysis of thick samples

Science.gov (United States)

Ali, Shad; Zeb, Johar; Ahad, Abdul; Ahmad, Ishfaq; Haneef, M.; Akbar, Jehan

2015-09-01

This paper describes the standardization of the proton-induced x-ray emission (PIXE) technique for finding the elemental composition of thick samples. For the standardization, three different samples of standard reference materials (SRMs) were analyzed using this technique and the data were compared with the already known data of these certified SRMs. These samples were selected in order to cover the maximum range of elements in the periodic table. Each sample was irradiated for three different values of collected beam charges at three different times. A proton beam of 2.57 MeV obtained using 5UDH-II Pelletron accelerator was used for excitation of x-rays from the sample. The acquired experimental data were analyzed using the GUPIXWIN software. The results show that the SRM data and the data obtained using the PIXE technique are in good agreement.

High performance liquid chromatographic hydrocarbon group-type analyses of mid-distillates employing fuel-derived fractions as standards

Science.gov (United States)

Seng, G. T.; Otterson, D. A.

1983-01-01

Two high performance liquid chromatographic (HPLC) methods have been developed for the determination of saturates, olefins and aromatics in petroleum and shale derived mid-distillate fuels. In one method the fuel to be analyzed is reacted with sulfuric acid, to remove a substantial portion of the aromatics, which provides a reacted fuel fraction for use in group type quantitation. The second involves the removal of a substantial portion of the saturates fraction from the HPLC system to permit the determination of olefin concentrations as low as 0.3 volume percent, and to improve the accuracy and precision of olefins determinations. Each method was evaluated using model compound mixtures and real fuel samples.

Liquid chromatographic-mass spectrometric method for ...

African Journals Online (AJOL)

Tropical Journal of Pharmaceutical Research ... Purpose: To develop and validate a simple, efficient and reliable Liquid chromatographic-mass spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs, ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

Standardization of P-33 by the TDCR efficiency calculation technique

CSIR Research Space (South Africa)

Simpson, BRS

2004-02-01

Full Text Available The activity of the pure beta-emitter phosphorus-33 (P-33) has been directly determined by the triple-to-double coincidence ratio (TDCR) efficiency calculation technique, thus extending the number of radionuclides that have been standardized...

Chromatographic efficiency of polar capillary columns applied for the analysis of fatty acid methyl esters by gas chromatography.

Science.gov (United States)

Waktola, Habtewold D; Mjøs, Svein A

2018-04-01

The chromatographic efficiency that could be achieved in temperature-programmed gas chromatography was compared for four capillary columns that are typically applied for analysis of fatty acid methyl esters (FAME). Three different carrier gases, hydrogen, helium and nitrogen, were applied. For each experiment, the carrier gas velocities and the temperature rates were varied with a full 9 × 3 design, with nine levels on the carrier gas velocity and temperature rates of 1, 2 or 3°C/min. Response surface methodology was used to create models of chromatographic efficiency as a function of temperature rate and carrier gas velocity. The chromatographic efficiency was defined as the inverse of peak widths measured in retention index units. The final results were standardized so that the efficiencies that could be achieved within a certain time frame, defined by the retention time of the last compound in the chromatogram, could be compared. The results show that there were clear differences in the efficiencies that could be achieved with the different columns and that the efficiency decreased with increasing polarity of the stationary phase. The differences can be explained by higher resistance to mass transfer in the stationary phase in the most polar columns. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-pressure liquid chromatographic determination of chlorphenesin carbamate and the beta-isomeric carbamate.

Science.gov (United States)

Beyer, W F

1976-12-01

A high-pressure liquid chromatographic assay was developed for the determination of chlorphenesin carbamate and its beta-isomeric carbamate. A single 4-mm i.d. X 30-cm column, prepacked with 10 micrometer fully porous silica gel particles, is used with 3% methanol in 50% water-saturated butyl chloride as the mobile phase. The procedure separates chlorphenesin carbamate from several possible impurities in addition to the beta-isomeric carbamate. The assay was applied to bulk drug and compressed tablets. The relative standard deviations for the assays of chlorphenesin carbamate and the beta-isomer are approximately 1 and 2%, respectively.

Analysis and chromatographic purification of eicosanoids multiply labeled by tritium

International Nuclear Information System (INIS)

Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

1989-01-01

We show the possibility of analysis and chromatographic purification of eicosanoids triply labeled by tritium. The described methods allow us to isolate chromatographically pure products obtained by selective hydrogenatin, chemical, and enzyme methods, with radiochemical purity at least 95-97%. The following methods are used to analyze the reaction mixtures and to isolate the tritium-labeled eicosanoids: gas-liquid chromatography, high-efficiency liquid chromatography, and thin-layer chromatography on supports impregnated with silver nitrate

Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

Science.gov (United States)

Valentin, J. R.

1989-01-01

Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

A Selective High Performance Liquid Chromatographic Method to Follow the Hydrolytic Degradation of Nicardipine Hydrochloride

Directory of Open Access Journals (Sweden)

K. E. Ibrahim

2010-01-01

Full Text Available A simple, stability indicating, reverse phase high performance liquid chromatographic method was developed and validated for determination of nicardipine hydrochloride (NC in the presence of its degradation products. The chromatographic separation was performed on Hypersil, BDS-C18, 30 cm × 3.9 mm id, at ambient temperature with UV-detection at 254 nm. A mixture of 20% (v/v aqueous 0.01 M sodium acetate∕acetic acid buffer (pH 4.5 and 80% acetonitrile was used as the mobile phase at a flow rate of 1.5 mL min-1, losartan was used as internal standard. The calibration curve is linear over the concentration range 5-40 μg mL-1, with a regression coefficient of 0.9984 and the % recovery was 99.78±0.17. The method was used to investigate the kinetics of alkaline, acids induced degradation, effect of buffer concentration and temperature. The degradation followed first-order kinetics. The rate constant, half-life time, and activation energy were calculated

Isotope separations using chromatographic methods

International Nuclear Information System (INIS)

Leseticky, L.

1985-01-01

A survey is given of chromatographic separations of compounds only differing in isotope composition. Isotope effects on physical properties which allow chromatographic separation (vapour tension, adsorption heat, partition coefficient) are very small, with the exception of the simplest molecules. Therefore, separation factors only assume the value of several per cent. From this ensues the necessity of using columns which are specially and very carefully prepared and have a separation efficiency of the order of 10 4 theoretical plates. Briefly discussed is liquid chromatography on ion exchangers which with a varied degree of success was used for separating simple inorganic compounds or ions. Ion exchange chromatography of amino acids labelled with tritium, and chromatography of tritium labelled steroids also provided only a certain degree of separation. A detailed analysis is presented of gas chromatography separation of various deuterium and tritium labelled low-molecular compounds, to which a number of studies has been devoted in the literature. Very promising is the method of complexation gas chromatography based on the reversible formation of a complex of the ligand (the compound being separated) and the compound of the (transition) metal as the steady-state phase. (author)

Rapid Analysis Procedures for Triglycerides and Fatty Acids as Pentyl and Phenethyl Esters for the Detection of Butter Adulteration Using Chromatographic Techniques

Directory of Open Access Journals (Sweden)

Daniele Naviglio

2017-01-01

Full Text Available This paper presents the development of three methods for quality control, fraud detection, and authentication of butter fat and other oils/fats using chromatographic techniques, with one method for triglycerides and two methods for fatty acids (FAs. The procedure for the analysis of triglycerides requires only dissolution of the sample in n-hexane and gas chromatography (GC analysis using a capillary column. The second method is based on the transesterification of triglycerides as pentyl esters in a single-step reaction using sodium pentanoate in pentanol. The reaction proceeds at room temperature and is similar to the potassium hydroxide-catalysed transesterification of triglycerides with methanol and even more similar to the sodium methoxide method and sodium butanoate method. The advantage of using pentyl esters includes reducing the volatility of short-chain FAs, and substantial recoveries were obtained compared with methyl ester analysis. The third method involves the transesterification of triglycerides in fat through reaction with 2-phenylethanol in a single step; 2-phenylethanol possesses a chromophore, and the phenethyl esters formed are analysed by high-performance liquid chromatography (HPLC with UV detection.

The development of an efficient mass balance approach for the purity assignment of organic calibration standards.

Science.gov (United States)

Davies, Stephen R; Alamgir, Mahiuddin; Chan, Benjamin K H; Dang, Thao; Jones, Kai; Krishnaswami, Maya; Luo, Yawen; Mitchell, Peter S R; Moawad, Michael; Swan, Hilton; Tarrant, Greg J

2015-10-01

The purity determination of organic calibration standards using the traditional mass balance approach is described. Demonstrated examples highlight the potential for bias in each measurement and the need to implement an approach that provides a cross-check for each result, affording fit for purpose purity values in a timely and cost-effective manner. Chromatographic techniques such as gas chromatography with flame ionisation detection (GC-FID) and high-performance liquid chromatography with UV detection (HPLC-UV), combined with mass and NMR spectroscopy, provide a detailed impurity profile allowing an efficient conversion of chromatographic peak areas into relative mass fractions, generally avoiding the need to calibrate each impurity present. For samples analysed by GC-FID, a conservative measurement uncertainty budget is described, including a component to cover potential variations in the response of each unidentified impurity. An alternative approach is also detailed in which extensive purification eliminates the detector response factor issue, facilitating the certification of a super-pure calibration standard which can be used to quantify the main component in less-pure candidate materials. This latter approach is particularly useful when applying HPLC analysis with UV detection. Key to the success of this approach is the application of both qualitative and quantitative (1)H NMR spectroscopy.

Chromatographic monitoring procedures in laboratory practice

Energy Technology Data Exchange (ETDEWEB)

Kaplina, E G; Belova, O I; Lasunina, N A

1976-01-01

The Moscow Coke and Chemical Works consist of three plants in combination, viz., the coking plant, the synthetic ammonia plant using coke-oven-gas hydrogen and the oxygen plant. The plant requirements include daily analyses not only of the coke-oven gas but also of a rich gas and an ethylene fraction. The analyses are carried out in VTI-2 apparatus. The analytical data are used to calculate the calorific values and densities of the gases. The time requirements are very considerable and the laboratory has long been engaged in developing and introducing chromatographic procedures for the major constituents of coke-oven gas, rich gas and ethylene fraction. The procedure developed for the coke-oven and rich gases uses two parallel columns, one packed with molecular sieves and the other with grade KSM silica gel. Hydrogen was determined with argon as the carrier gas, and all other constituents with helium. The procedure was time-consuming and complicated. An attempt was made to separate the gases in an LKhM-7a chromatograph with a programme-controlled 50 to 250/sup 0/C heating cycle, but the procedure still had a number of serious defects and could not be recommended for regular quality control. The final variant involved two parallel columns and a procedure based on that in GOST 14920 (''Dry gas. Proximate analysis''). The chromatograph was a type KhL-69 with a 6-way cock in the gas line so that each of the columns could be brought on stream in succession. The analytical column packings were zeolite (in a 2 m column) and diatomaceous brick with 25% n-hexadecane (in a 6 m column).

Use of coextraction and suppression of extraction in extraction-chromatographic separation of elements

International Nuclear Information System (INIS)

Karandashev, V.K.; Kuznetsov, R.A.; Grazhulene, S.S.; Usmanova, M.M.

1988-01-01

TBP, solutions of hydrobromic acid, indium and polytetrafluoroethylene powder, carrier for TBP, were used to study the effects of coextraction and extraction suppression on extraction-chromatographic behaviour of microamounts of elements in the presence of macroamounts of other elements. Possibility of using these effects under extraction-chromatographic element separation were considered. A new method for extraction-chromatographic separation of scandium microamounts from the mixture of large amount of elements (Y, Cd, Ce, Eu, Lu, Hf, Ta, W, Np and other) was suggested. 15 refs.; 3 figs

Liquid chromatographic separation of zalcitabine and its stereoisomers.

Science.gov (United States)

Scypinski, S; Ross, A J

1994-10-01

A liquid chromatographic method capable of separating and quantitating the stereoisomers of zalcitabine has been developed and validated. The separation was achieved with an Astec Cyclobond I--RSP column and a mobile phase of 0.25% triethylamine in water adjusted to a pH of 6.5 with glacial acetic acid. All enantiomers were found to exhibit a linear response in the range of 0.1-10% in the presence of 100% zalcitabine. Precision of analysis was found to be less than 1.5% at a level of 1% relative to zalcitabine. The limit of detection for two of the three enantiomeric impurities was determined to be 0.05% relative to zalcitabine. The detection limit for the third was found to be 0.1%. This method was successfully applied to the analysis of reference standards and several production scale batches. All of these materials were found to be stereochemically pure to a level of 99.8% or better.

Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

OpenAIRE

Nataša Gros

2013-01-01

This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as com...

Chromatographic decontamination of medium-activity waste concentrates

International Nuclear Information System (INIS)

Faubel, W.; Menzler, P.M.; Sameh, A.A.

1988-01-01

The chromatographic decontamination of a MAW concentrate was carried out in a laboratory plant in 1-l-batches in the following way: In order to purify the nitric MAW concentrate from its solid and organic contamination products, it is passed through a filter and an absorber (SM7) for organic species. Subsequently the purified solution runs on-line through all following columns. First the main activity carrier cesium ( 137 Cs, 134 Cs) is transferred to ammonium molybdate phosphate (AMP-1) by means of a newly developed fluidized bed process. In the further course, 125 Sb is separated on metal oxides (Sb 2 O 5 , MnO 2 ) and the three-valued actinides/lanthanides on an extraction-chromatographic CMPO column. Finally the remaining 106 Ru and 60 Co activities are separated on dimethylglyoximes (DMG) coated on active carbon. (orig./RB) [de

Pyrolysis-gas chromatographic method for kerogen typing

Energy Technology Data Exchange (ETDEWEB)

Larter, S.R.; Douglas, A.G.

1980-01-01

The classification of kerogens according to their type and rank is important for the definition of any kerogen assemblage. Whereas optical methods of rank determination are well known, vitrinite reflectance and spore coloration being the most widely accepted chemical methods for typing kerogens are less developed. In this work we show that pyrograms, produced by pyrolyzing microgram quantities of solvent-extracted kerogens, enable not only their characterization in terms of a chromatographic fingerprint but also the production of a numerical type index determined as the ratio of m(+p)-xylene/n-octene (oct-1-ene) in the pyrogram. This index appears to be a close function of kerogen type. Type 3 kerogens (Tissot et al., 1974), including vitrinite, provide a high type index and have pyrolysates dominated by aromatic and phenolic compounds whereas type 1 kerogens provide an aliphatic-rich pyrolysate and consequently a low type index. The type index described here correlates well with microscopic and elemental analysis data and the pyrogram fingerprint provides an additional level of characterization not attainable with other current typing techniques.

HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC DETERMINATION OF CAFFEIC ACID AND ROSMARINIC ACID FROM THE LEAVES OF Orthosiphon stamineus

Directory of Open Access Journals (Sweden)

M. Amzad Hossain

2010-06-01

Full Text Available This paper presents the studies performed on extraction of Orthosiphon stamineus, Benth by using different solvent for the identification and quantification of the caffeic acid derivatives such as caffeic acid  and rosmarinic acid which confers to the leaves of this plant with remarkable pharmaceutical properties. High performance thin-layer chromatographic (HPTLC allows the identification and the quantification of more than 20 samples in the same chromatographic run. The analysis of the samples requires 15-30 min compared with more than 2 h using a typical HPLC method. Using the techniques of the HPTLC and the UV-VIS spectra we have found that the extraction of this herb plant contain, the caffeic acid and rosmarinic acid ranging between 0.029% up to 0.506% and up to 0.24% to 2.24% respectively.     Keywords: Caffice acid derivatives, quantification, Malaysian Orthosiphon stamineus, HPTLC

Preparation and certification of solutions of perdeuterated polycyclic aromatic compounds intended for use as surrogate internal standards

International Nuclear Information System (INIS)

Quilliam, M.A.; Hardstaff, W.R.; Anacleto, J.F.; LeBlanc, M.D.; Stergiopoulos, V.; Dick, K.L.; Bowser, M.T.; Curtis, J.M.; Embree, D.J.; Sim, P.G.; Boyd, R.K.

1994-01-01

Two standard solutions of deuterated polycyclic aromatic compounds (PACs) have been prepared for use as surrogate internal standards. Solution DPAC-1 contains 21 deuterated PACs, and is intended for use with mass spectrometric (MS) detection. Most of the difficulties in certifying concentrations in DPAC-1 arose from the fact that none of the individual compounds was 100% deuterated, so that effects of mass spectrometric fragmentation are convoluted with those of isotopic distributions. The best methods are discussed for using such internal standards so as to minimize these problems, together with those arising from kinetic isotope effects. Solution DPAC-2 contains 6 deuterated PACs, and is primarily intended for use with reversed-phase high-performance liquid chromatography (HPLC) with fluorescence detection (FLD, dural programmed wavelength mode), in which the signals for analyte and internal standard are separated chromatographically rather than via the detector. Full details of the preparation of these solutions are described. In addition, examples of their use in the analysis of a certified coal-tar extract (NIST SRM 1597) are described briefly. In one example a novel HPLC-MS technique was employed, and in the other the HPLC-FLD technique was used. (orig.)

Research on technology of online gas chromatograph for SF6 decomposition products

Science.gov (United States)

Li, L.; Fan, X. P.; Zhou, Y. Y.; Tang, N.; Zou, Z. L.; Liu, M. Z.; Huang, G. J.

2017-12-01

Sulfur hexafluoride (SF6) decomposition products were qualitatively and quantitatively analyzed by several gas chromatographs in the laboratory. Test conditions and methods were selected and optimized to minimize and eliminate the SF6’ influences on detection of other trace components. The effective separation and detection of selected characteristic gases were achieved. And by comparison among different types of gas chromatograph, it was found that GPTR-S101 can effectively separate and detect SF6 decomposition products and has best the best detection limit and sensitivity. On the basis of GPTR-S101, online gas chromatograph for SF6decomposition products (GPTR-S201) was developed. It lays the foundation for further online monitoring and diagnosis of SF6.

High-pressure liquid chromatographic assay of Bay n 7133 in human serum.

OpenAIRE

Fasching, C E; Hughes, C E; Hector, R F; Peterson, L R

1984-01-01

A high-pressure liquid chromatographic method that includes a Sep-Pak (Waters Associates, Inc., Milford , Mass.) preparation of human serum was employed for the quantitative assay of Bay n 7133. Drug levels of 0.1 to 20 micrograms/ml could be detected. No interference from amphotericin B was found in the chromatographic analysis of Bay n 7133.

Confocal Raman Microscopy for in Situ Measurement of Phospholipid-Water Partitioning into Model Phospholipid Bilayers within Individual Chromatographic Particles.

Science.gov (United States)

Kitt, Jay P; Bryce, David A; Minteer, Shelley D; Harris, Joel M

2018-06-05

The phospholipid-water partition coefficient is a commonly measured parameter that correlates with drug efficacy, small-molecule toxicity, and accumulation of molecules in biological systems in the environment. Despite the utility of this parameter, methods for measuring phospholipid-water partition coefficients are limited. This is due to the difficulty of making quantitative measurements in vesicle membranes or supported phospholipid bilayers, both of which are small-volume phases that challenge the sensitivity of many analytical techniques. In this work, we employ in situ confocal Raman microscopy to probe the partitioning of a model membrane-active compound, 2-(4-isobutylphenyl) propionic acid or ibuprofen, into both hybrid- and supported-phospholipid bilayers deposited on the pore walls of individual chromatographic particles. The large surface-area-to-volume ratio of chromatographic silica allows interrogation of a significant lipid bilayer area within a very small volume. The local phospholipid concentration within a confocal probe volume inside the particle can be as high as 0.5 M, which overcomes the sensitivity limitations of making measurements in the limited membrane areas of single vesicles or planar supported bilayers. Quantitative determination of ibuprofen partitioning is achieved by using the phospholipid acyl-chains of the within-particle bilayer as an internal standard. This approach is tested for measurements of pH-dependent partitioning of ibuprofen into both hybrid-lipid and supported-lipid bilayers within silica particles, and the results are compared with octanol-water partitioning and with partitioning into individual optically trapped phospholipid vesicle membranes. Additionally, the impact of ibuprofen partitioning on bilayer structure is evaluated for both within-particle model membranes and compared with the structural impacts of partitioning into vesicle lipid bilayers.

Pyrolysis gas chromatographic atomic emission detection for sediments, coals and other petrochemical precursors

Energy Technology Data Exchange (ETDEWEB)

Seeley, J.A.; Zeng, Y.D.; Uden, P.C.; Eglinton, T.I.; Ericson, I. (Massachusetts University, Amherst, MA (USA). Dept. of Chemistry)

1992-09-01

On-line flash pyrolysis coupled to a capillary gas chromatograph for the characterization of marine sediments, coals and other heterogeneous solid samples is described. A helium microwave-induced plasma is used for chromatographic detection by atomic emission spectrometry. Simultaneous multi-element detection is achieved with a photodiode array detector. The optical path of the gas chromatographic atomic emission detector is purged with helium, allowing simultaneous, sensitive detection of atomic emission from sulfur 181 nm, phosphorous 186 nm, arsenic 189 nm, selenium 196 nm and carbon 193 nm. Several sediment and coal samples have been analysed for their carbon, nitrogen, sulfur, oxygen, phosphorous, arsenic and selenium content. Qualitative information indicating the occurrence and distribution of these elements in the samples can be used to gauge the relative stage of diagenetic evolution of the samples and provide information on their depositional environment. In some instances the chromatographic behaviour of the compounds produced upon pyrolysis is improved through on-line alkylation. This on-line derivatization is achieved by adding liquid reagents to the pyrolysis probe or by adding liquid reagents to the pyrolysis probe or by adding solid reagents either to the solid sample or by packing the reagent in the injection port of the chromatograph.

Dimethylthioarsinic anhydride: A standard for arsenic speciation

International Nuclear Information System (INIS)

Fricke, Michael; Zeller, Matthias; Cullen, William; Witkowski, Mark; Creed, John

2007-01-01

Dimethylthioarsinic acid (DMTA V ) has recently been identified in biological, dietary and environmental matrices. The relevance of this compound to the toxicity of arsenic in humans is unknown and further exposure assessment and metabolic studies are difficult to conduct because of the unavailability of a well characterized standard. The synthesis of DMTA V was accomplished by the reaction of dimethylarsinic acid (DMA V ) with hydrogen sulfide. The initial reaction product produced is DMTA V but multiple products over the course of the reaction are also observed. Therefore, a chromatographic separation was developed to monitor the reaction progress via LC-ICP-MS. In this synthesis, conversion of DMA V to DMTA V was not taken to completion to avoid the production of side products. The product was isolated from the starting material by standard organic techniques. Single crystal diffraction demonstrated that solid DMTA V is present in the form of the oxygen-bridged dimethylthioarsinic anhydride. Dissolution of the anhydride in water produces the acid form of DMTA V and the aqueous phase DMTA V provided a characteristic molecular ion of m/z 155 by LC-ESI-MS. The synthesis and isolation of dimethylthioarsinic anhydride provides a stable crystalline standard suitable for identification, toxicological study and exposure assessment of dimethylthioarsinic acid

Chromatographic generator systems for the actinides and natural decay series elements

International Nuclear Information System (INIS)

McAlister, D.R.; Horwitz, E.P.

2011-01-01

This work describes chromatographic radionuclide generator systems for the production of actinides and natural decay series elements. The generator systems begin with alpha emitting parent radioisotopes with half-lives (T 1/2 ) of greater than one year and produce alpha or beta emitting radioisotopes with half-lives of hours to days. Chromatographic systems were chosen to minimize radiolytic damage to chromatographic supports, preserve the parent activity for repeated use, provide high purity daughter radionuclide tracers, and to minimize or eliminate the need for evaporation of solutions of the parent or daughter nuclides. Useful secondary separations involving the daughters of the initial parent radionuclide are also described. Separation systems for 210 Bi, 210 Po, 211 Pb, 212 Pb, 223 Ra, 224 Ra, 225 Ra, 225 Ac, 227 Th, 228 Th, 231 Th, 234 Th, and 239 Np are outlined in detail. (orig.)

Best-Matched Internal Standard Normalization in Liquid Chromatography-Mass Spectrometry Metabolomics Applied to Environmental Samples.

Science.gov (United States)

Boysen, Angela K; Heal, Katherine R; Carlson, Laura T; Ingalls, Anitra E

2018-01-16

The goal of metabolomics is to measure the entire range of small organic molecules in biological samples. In liquid chromatography-mass spectrometry-based metabolomics, formidable analytical challenges remain in removing the nonbiological factors that affect chromatographic peak areas. These factors include sample matrix-induced ion suppression, chromatographic quality, and analytical drift. The combination of these factors is referred to as obscuring variation. Some metabolomics samples can exhibit intense obscuring variation due to matrix-induced ion suppression, rendering large amounts of data unreliable and difficult to interpret. Existing normalization techniques have limited applicability to these sample types. Here we present a data normalization method to minimize the effects of obscuring variation. We normalize peak areas using a batch-specific normalization process, which matches measured metabolites with isotope-labeled internal standards that behave similarly during the analysis. This method, called best-matched internal standard (B-MIS) normalization, can be applied to targeted or untargeted metabolomics data sets and yields relative concentrations. We evaluate and demonstrate the utility of B-MIS normalization using marine environmental samples and laboratory grown cultures of phytoplankton. In untargeted analyses, B-MIS normalization allowed for inclusion of mass features in downstream analyses that would have been considered unreliable without normalization due to obscuring variation. B-MIS normalization for targeted or untargeted metabolomics is freely available at https://github.com/IngallsLabUW/B-MIS-normalization .

Chromatographic background drift correction coupled with parallel factor analysis to resolve coelution problems in three-dimensional chromatographic data: quantification of eleven antibiotics in tap water samples by high-performance liquid chromatography coupled with a diode array detector.

Science.gov (United States)

Yu, Yong-Jie; Wu, Hai-Long; Fu, Hai-Yan; Zhao, Juan; Li, Yuan-Na; Li, Shu-Fang; Kang, Chao; Yu, Ru-Qin

2013-08-09

Chromatographic background drift correction has been an important field of research in chromatographic analysis. In the present work, orthogonal spectral space projection for background drift correction of three-dimensional chromatographic data was described in detail and combined with parallel factor analysis (PARAFAC) to resolve overlapped chromatographic peaks and obtain the second-order advantage. This strategy was verified by simulated chromatographic data and afforded significant improvement in quantitative results. Finally, this strategy was successfully utilized to quantify eleven antibiotics in tap water samples. Compared with the traditional methodology of introducing excessive factors for the PARAFAC model to eliminate the effect of background drift, clear improvement in the quantitative performance of PARAFAC was observed after background drift correction by orthogonal spectral space projection. Copyright © 2013 Elsevier B.V. All rights reserved.

Industrial scale chromatographic separation of valuable compounds from biomass hydrolysates and side streams

Energy Technology Data Exchange (ETDEWEB)

Saari, P.

2011-06-15

Carbohydrates are composed of a number of various monosaccharides, glucose being the most abundant. Some of the monosaccharides are valuable compounds used in the food and pharmaceutical industries. They can be separated from biomass hydrolysates e.g. by chromatographic methods. In this thesis, chromatographic separation of valuable compounds using ion exchange resins was studied on an industrial scale. Of special interest were rare monosaccharides in biomass hydrolysates. A novel chromatographic separation process was developed for fucose, starting from pre-processed spent sulfite liquor. The core of the process consists of three chromatographic separations with different types of ion exchange resins. Chromatographic separation of galactose was tested with three biomass hydrolysates; lactose, gum arabic and hemicellulose hydrolysates. It was demonstrated that also galactose can be separated from complex carbohydrate mixtures. A recovery process for arabinose from citrus pectin liquid residual and for mannose from wood pulp hydrolysate were also developed and experimentally verified. In addition to monosaccharides, chromatographic separation of glycinebetaine from vinasse was examined with a hydrogen form weak acid cation exchange resin. The separation involves untypical peak formation depending, for example, on the pH and the cation composition. The retention mechanism was found to be hydrogen bonding between glycinebetaine and the resin. In the experimental part, all four resin types - strong acid cation, strong base anion, weak acid cation and weak base anion exchange resins - were used. In addition, adsorption equilibria data of seven monosaccharides and sucrose were measured with the resins in sodium and sulfate forms because such data have been lacking. It was found out that the isotherms of all sugars were linear under industrial conditions. A systematic method for conceptual process design and sequencing of chromatographic separation steps were developed

Chromatographic separation of low-temperature tar. Part II

Energy Technology Data Exchange (ETDEWEB)

Terres, E; Gebert, F; Huelsemann, H; Petereit, H; Toepsch, H; Ruppert, W

1955-01-01

Chromatographic methods and apparatus are discussed. The Folin-Denis reagent (Na tungstate molybdate in H/sub 3/PO/sub 4/) is used for developing paper chromatograms of phenol mixtures. Other reagents are given.

Quantitative Mass Spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

Directory of Open Access Journals (Sweden)

Nahla N. Salama

2009-01-01

Full Text Available The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL −1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%-102.75% was obtained. The method is accurate (% RE <; 5% and reproducible with intra- and inter-assay precision (RSD% <; 8.0%. The quantification limit is 23.8 ng mL −1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

Quantitative Mass spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

Directory of Open Access Journals (Sweden)

Nahla N. Salama

2009-01-01

Full Text Available The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL-1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%–102.75% was obtained. The method is accurate (% RE < 5% and reproducible with intra- and inter-assay precision (RSD% < 8.0%. The quantification limit is 23.8 ng mL-1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

The behaviour of radionuclides in gas adsorption chromatographic processes with superimposed chemical reactions (chlorides)

International Nuclear Information System (INIS)

Eichler, B.

1996-01-01

Thermochemical relationships are derived describing the gas adsorption chromatographic transport of carrier-free radionuclides. Especially, complex adsorption processes such as dissociative, associative and substitutive adsorption are dealt with. The comparison of experimental with calculated data allows the determination of the type of adsorption reaction, which is the basis of the respective gas chromatographic process. The behaviour of carrier-free radionuclides of elements Pu, Ce, Ru, Co and Cr in thermochromatographic experiments with chlorinating carrier gases can be described as dissociative adsorption of chlorides in higher oxidation states. The gas adsorption chromatographic transport of Zr with oxygen and chlorine containing carrier gas is shown to be a substitutive adsorption process. The consequences of superimposed chemical reactions on the interpretation of results and the conception of gas adsorption chromatographic experiments with carrier-free radionuclides in isothermal columns and in temperature gradient tubes is discussed. (orig.)

Chromatographic characterisation, in vitro antioxidant and free ...

African Journals Online (AJOL)

Chromatographic fractionation and spectroscopic analysis of the ME4 fraction revealed the presence of four compounds namely garcinia biflavonoids GB1 and GB2, garcinal and garcinoic acid. These findings show that these four compounds are partly responsible for the great antioxidant potential of G. kola seeds.

Gas-chromatographic separation of hydrogen isotopic mixtures

International Nuclear Information System (INIS)

Preda, Anisoara; Bidica, Nicolae

2005-01-01

Full text: Gas chromatographic separation of hydrogen isotopes have been reported in the literature since late of 1950's. Gas chromatography is primarily an analytical method, but because of its properties it may be used in many other fields with excellent results. A simple method is proposed for the gas-chromatographic analysis of complex gas mixtures containing hydrogen isotopes; the method is based on the substantial difference in the thermal conductivity of these isotopes. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures while the column is operated at very low temperature. The method described in this paper was based on using a capillary molecular sieve 5A column operated for this kind of separation at 173 K. The carrier gas was Ne and the detector was TCD. In the paper chromatograms for various carrier flow rates and various hydrogen isotope mixtures are presented. (authors)

Direct coupling of a dense (supercritical) gas chromatograph to a mass spectrometer using a supersonic molecular beam interface

International Nuclear Information System (INIS)

Randall, L.G.; Wahrhaftig, A.L.

1981-01-01

A detecting mass spectrometer has been successfully coupled to a dense gas (supercritical fluid) chromatograph to produce an instrument (DGC/MS) that may be an alternative to high performance liquid chromatograph/mass spectrometer instruments (HPLC/MS) and gas chromatograph/mass spectrometer instruments (GC/MS) for analysis of involatile and/or thermally labile compounds. The mobile phase in DGC is a gas held at temperatures above the critical temperature and at pressures sufficient to obtain nearly liquid-like densities. DGC combines advantages of GC and HPLC: rapid separations, moderate operating temperatures, and analysis of involatile compounds. An advantage unique to DGC is the solvent power dependence upon pressure. While several groups have studied DGC, its development has been limited by the lack of a sensitive and selective detector. Hence, work has been directed towards the design and construction of a DGC/MS resulting in a trial instrument capable of chromatographic pressures of at least 300 atm and temperatures from 10 0 to 60 0 C. The DGC/MS coupling has been accomplished by the use of a supersonic molecular beam interface. This application of molecular beam formation appears to be unique in its requirements of a large pressure ratio (approx.10 8 ), low flow rates, and low final pressures. The authors outline characteristics of supersonic jets and molecular beams pertinent to the design of such an instrument. The interface which uses pumping speeds of 2400 and 1200 l/s in the beam forming chambers is described in detail, while the other components: the detecting mass spectrometer, the dense gas supply, and the DGC: are briefly described. Preliminary work with this instrument has established the feasibility of DGC/MS as an analytical technique and further development is recommended

A review of chromatographic methods for the determination of water- and fat-soluble vitamins in biological fluids.

Science.gov (United States)

Karaźniewicz-Łada, Marta; Główka, Anna

2016-01-01

Vitamins are an essential element of nutrition and thus contribute to human health. Vitamins catalyze many biochemical reactions and their lack or excess can cause health problems. Therefore, monitoring vitamin concentrations in plasma or other biological fluids may be useful in the diagnosis of various disorders as well as in the treatment process. Several chromatographic methods have been developed for the determination of these compounds in biological samples, including high-performance liquid chromatography with UV and fluorescence detection. Recently, high-performance liquid chromatography with tandem mass spectrometry methods have been widely used for the determination of vitamins in complex matrices because of their high sensitivity and selectivity. This method requires preconditioning of samples for analysis, including protein precipitation and/or various extraction techniques. The choice of method may depend on the desired cost, convenience, turnaround time, specificity, and accuracy of the information to be obtained. This article reviews the recently reported chromatographic methods used for determination of vitamins in biological fluids. Relevant papers published mostly during the last 5 years were identified by an extensive PubMed search using appropriate keywords. Particular attention was given to the preparation steps and extraction techniques. This report may be helpful in the selection of procedures that are appropriate for certain types of biological materials and analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chromatographic Methods for the Analysis of Polyphenols in Wines

Directory of Open Access Journals (Sweden)

Medić-Šarić, M.

2009-03-01

Full Text Available Wine is an excellent source of various classes of polyphenols, including phenolic acids, flavonoids, and trihydroxystilbene resveratrol (Fig.1. Polyphenols play a major role in wine quality since they contribute to the sensory characteristics of wine, particularly color and astringency. A recent interest in these substances has been stimulated by abundant evidence of their beneficial effects on human health, such as anticarcinogenic, antiinflamatory and antimicrobial activities. Therefore, numerous studies have been performed in the attempt to analyze polyphenols in wine. This paper reviews the current advances in the determination of polyphenols in wine by the major chromatographic techniques such as thin-layer chromatography (TLC and high-performance liquid chromatography (HPLC.The great complexity of the polyphenolic content of wine and the difficulty in obtaining some of the standards usually require sample preparation before analysis. Two methods for sample preparation, liquid-liquid extraction and solid-phase extraction, are most commonly applied. Hydrolysis is applied frequently, but not exclusively, to remove the sugar moieties from glycosides.TLC on silica gel plates is useful for the rapid and low-cost separation and identification of the polyphenols present in wine (Fig. 2. Densitometric quantitative analysis of polyphenols in wine extracts is usually performed by scanning the TLC plates with UV light at wavelengths of 350–365 nm or 250–260 nm (Fig. 3. For the evaluation of the most efficient mobile phase and an optimal choice of the combination of two or more mobile phases, two methods may be applied: information theory and numerical taxonomy. HPLC currently represents the most popular technique for the analysis of polyphenols in wine. For this purpose, a reversed-phase HPLC method that uses gradient elution with binary elution system is usually employed. Routine detection is based on measurement of UV-Vis absorption with a diode

Validated high performance liquid chromatographic (HPLC) method ...

African Journals Online (AJOL)

STORAGESEVER

2010-02-22

Feb 22, 2010 ... specific and accurate high performance liquid chromatographic method for determination of ZER in micro-volumes ... tional medicine as a cure for swelling, sores, loss of appetite and ... Receptor Activator for Nuclear Factor κ B Ligand .... The effect of ... be suitable for preclinical pharmacokinetic studies. The.

Development, enhancement, and evaluation of aircraft measurement techniques for national ambient air quality standard criteria pollutants

Science.gov (United States)

Brent, Lacey Cluff

The atmospheric contaminants most harmful to human health are designated Criteria Pollutants. To help Maryland attain the national ambient air quality standards (NAAQS) for Criteria Pollutants, and to improve our fundamental understanding of atmospheric chemistry, I conducted aircraft measurements in the Regional Atmospheric Measurement Modeling Prediction Program (RAMMPP). These data are used to evaluate model simulations and satellite observations. I developed techniques for improving airborne observation of two NAAQS pollutants, particulate matter (PM) and nitrogen dioxide (NO2). While structure and composition of organic aerosol are important for understanding PM formation, the molecular speciation of organic ambient aerosol remains largely unknown. The spatial distribution of reactive nitrogen is likewise poorly constrained. To examine water-soluble organic aerosol (WSOA) during an air pollution episode, I designed and implemented a shrouded aerosol inlet system to collect PM onto quartz fiber filters from a Cessna 402 research aircraft. Inlet evaluation conducted during a side-by-side flight with the NASA P3 demonstrated agreement to within 30%. An ion chromatographic mass spectrometric method developed using the NIST Standard Reference Material (SRM) 1649b Urban Dust, as a surrogate material resulted in acidic class separation and resolution of at least 34 organic acids; detection limits approach pg/g concentrations. Analysis of aircraft filter samples resulted in detection of 8 inorganic species and 16 organic acids of which 12 were quantified. Aged, re-circulated metropolitan air showed a greater number of dicarboxylic acids compared to air recently transported from the west. While the NAAQS for NO2 is rarely exceeded, it is a precursor molecule for ozone, America's most recalcitrant pollutant. Using cavity ringdown spectroscopy employing a light emitting diode (LED), I measured vertical profiles of NO2 (surface to 2.5 km) west (upwind) of the Baltimore

Identification of homemade inorganic explosives by ion chromatographic analysis of post-blast residues.

Science.gov (United States)

Johns, Cameron; Shellie, Robert A; Potter, Oscar G; O'Reilly, John W; Hutchinson, Joseph P; Guijt, Rosanne M; Breadmore, Michael C; Hilder, Emily F; Dicinoski, Greg W; Haddad, Paul R

2008-02-29

Anions and cations of interest for the post-blast identification of homemade inorganic explosives were separated and detected by ion chromatographic (IC) methods. The ionic analytes used for identification of explosives in this study comprised 18 anions (acetate, benzoate, bromate, carbonate, chlorate, chloride, chlorite, chromate, cyanate, fluoride, formate, nitrate, nitrite, perchlorate, phosphate, sulfate, thiocyanate and thiosulfate) and 12 cations (ammonium, barium(II), calcium(II), chromium(III), ethylammonium, magnesium(II), manganese(II), methylammonium, potassium(I), sodium(I), strontium(II), and zinc(II)). Two IC separations are presented, using suppressed IC on a Dionex AS20 column with potassium hydroxide as eluent for anions, and non-suppressed IC for cations using a Dionex SCS 1 column with oxalic acid/acetonitrile as eluent. Conductivity detection was used in both cases. Detection limits for anions were in the range 2-27.4ppb, and for cations were in the range 13-115ppb. These methods allowed the explosive residue ions to be identified and separated from background ions likely to be present in the environment. Linearity (over a calibration range of 0.05-50ppm) was evaluated for both methods, with r(2) values ranging from 0.9889 to 1.000. Reproducibility over 10 consecutive injections of a 5ppm standard ranged from 0.01 to 0.22% relative standard deviation (RSD) for retention time and 0.29 to 2.16%RSD for peak area. The anion and cation separations were performed simultaneously by using two Dionex ICS-2000 chromatographs served by a single autoinjector. The efficacy of the developed methods was demonstrated by analysis of residue samples taken from witness plates and soils collected following the controlled detonation of a series of different inorganic homemade explosives. The results obtained were also confirmed by parallel analysis of the same samples by capillary electrophoresis (CE) with excellent agreement being obtained.

Improvement in gradient ion chromatographic method for trace anions and organic acids in the PWR nuclear power plant

International Nuclear Information System (INIS)

Junlowjiraya, V.

1989-01-01

In a nuclear power plant the use of high quality water is very important to minimize corrosion and downtime of a plant system. To evaluate the quality of water the most widely used instrument is a conductivity analyzer. However, conductivity monitor is nonspecific, the conductivity signal cannot give information about what species or impurities are presented in the water, steam, and condensate. To determine these impurities qualitatively and quantitatively, the ion chromatography is an effective technique. This presentation demonstrates an improvement of gradient ion chromatographic technique to solve lithium interference in the borated samples. The data acquisition system and computer automation setup for the analysis are also discussed

Standardization of MIP technique in three-dimensional CT portography: usefulness in evaluation of portosystemic collaterals in cirrhotic patients

International Nuclear Information System (INIS)

Kim, Jong Gi; Kim, Yong; Kim, Chang Won; Lee, Jun Woo; Lee, Suk Hong

2003-01-01

To assess the usefulness of three-dimensional CT portography using a standardized maximum intensity projection (MIP) technique for the evaluation of portosystemic collaterals in cirrhotic patients. In 25 cirrhotic patients with portosystemic collaterals, three-phase CT using a multide-tector-row helical CT scanner was performed to evaluate liver disease. Late arterial-phase images were transferred to an Advantage Windows 3.1 workstation (Gener Electric). Axial images were reconstructed by means of three-dimensional CT portography, using both a standardized and a non-standardized MIP technique, and the respective reconstruction times were determined. Three-dimensional CT portography with the standardized technique involved eight planes, namely the spleno-portal confluence axis (coronal, lordotic coronal, lordotic coronal RAO 30 .deg. C, and lordotic coronal LAO 30 .deg. C), the left renal vein axis (lordotic coronal), and axial MIP images (lower esophagus level, gastric fundus level and splenic hilum). The eight MIP images obtained in each case were interpreted by two radiologists, who reached a consensus in their evaluation. The portosystemic collaterals evaluated were as follows: left gastric vein dilatation; esophageal, paraesophageal, gastric, and splenic varix; paraumbilical vein dilatation; gastro-renal, spleno-renal, and gastro-spleno-renal shunt; mesenteric, retroperitoneal, and omental collaterals. The average reconstruction time using the non-standardized MIP technique was 11 minutes 23 seconds, and with the standardized technique, the time was 6 minutes 5 seconds. Three-dimensional CT portography with the standardized technique demonstrated left gastric vein dilatation (n=25), esophageal varix (n=18), paraesophageal varix (n=13), gastric varix (n=4), splenic varix (n=4), paraumbilical vein dilatation (n=4), gastro-renal shunt (n=3), spleno-renal shunt (n=3), and gastro-spleno-renal shunt (n=1). Using three-dimensional CT protography and the non-standardized

Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

Science.gov (United States)

Mills, G A; Walker, V

2000-12-01

Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

Characterization of plant polysaccharides from Dendrobium officinale by multiple chromatographic and mass spectrometric techniques.

Science.gov (United States)

Ma, Huiying; Zhang, Keke; Jiang, Qing; Dai, Diya; Li, Hongli; Bi, Wentao; Chen, David Da Yong

2018-04-27

Plant polysaccharides have numerous medicinal functions. Due to the differences in their origins, regions of production, and cultivation conditions, the quality and the functions of polysaccharides can vary significantly. They are macromolecules with large molecular weight (MW) and complex structure, and pose great challenge for the analytical technology used. Taking Dendrobium officinale (DO) from various origins and locations as model samples. In this investigation, mechanochemical extraction method was used to successfully extract polysaccharides from DO using water as solvent, the process is simple, fast (40 s) and with high yield. The MWs of the intact saccharides from calibration curve and light scattering measurement were determined and compared after separation with size exclusion chromatography (SEC). The large polysaccharide was acid hydrolyzed to oligosaccharides and the products were efficiently separated and identified using liquid chromatography coupled to a high resolution tandem mass spectrometry (LC-MS 2 ). Obvious differences were observed among LC-MS 2 chromatograms of digested products, and the chemical structures for the products were proposed based on accurate mass values. More importantly, isomeric digested carbohydrate compounds were explored and characterized. All the chromatographic and mass spectrometric results in this study provided a multi-dimensional characterization, fingerprint analysis, and molecular structure level assessment of plant polysaccharides. Copyright © 2018 Elsevier B.V. All rights reserved.

GAS CHROMATOGRAPHIC AND SPECTROSCOPIC ANALYSIS OF ...

African Journals Online (AJOL)

Peroxyformic acid prepared in-situ was employed for epoxidation of canola oil in the presence of toluene. Gas chromatographic analysis of the product revealed the following species: C16:0; C18:0; C18:1; C18:2; C18:3; monoepoxy C18:0; monoepoxy C18:1; monoepoxy C18:2; diepoxy C18:0; diepoxy C18:1 and triepoxy ...

Standardized technique for single port laparoscopic ileostomy and colostomy.

Science.gov (United States)

Shah, A; Moftah, M; Hadi Nahar Al-Furaji, H; Cahill, R A

2014-07-01

Single site laparoscopic techniques and technology exploit maximum usefulness from confined incisions. The formation of an ileostomy or colostomy seems very applicable for this modality as the stoma occupies the solitary incision obviating any additional wounds. Here we detail the principles of our approach to defunctioning loop stoma formation using single port laparoscopic access in a stepwise and standardized fashion along with the salient specifics of five illustrative patients. No specialized instrumentation is required and the single access platform is established table-side using the 'glove port' technique. The approach has the intra-operative advantage of excellent visualization of the correct intestinal segment for exteriorization along with direct visual control of its extraction to avoid twisting. Postoperatively, abdominal wall trauma has been minimal allowing convalescence and stoma care education with only one parietal incision. Single incision stoma siting proves a ready, robust and reliable technique for diversion ileostomy and colostomy with a minimum of operative trauma for the patient. Colorectal Disease © 2014 The Association of Coloproctology of Great Britain and Ireland.

Artificial neural network model for photosynthetic pigments identification using multi wavelength chromatographic data

Science.gov (United States)

Prilianti, K. R.; Hariyanto, S.; Natali, F. D. D.; Indriatmoko, Adhiwibawa, M. A. S.; Limantara, L.; Brotosudarmo, T. H. P.

2016-04-01

The development of rapid and automatic pigment characterization method become an important issue due to the fact that there are only less than 1% of plant pigments in the earth have been explored. In this research, a mathematical model based on artificial intelligence approach was developed to simplify and accelerate pigment characterization process from HPLC (high-performance liquid chromatography) procedure. HPLC is a widely used technique to separate and identify pigments in a mixture. Input of the model is chromatographic data from HPLC device and output of the model is a list of pigments which is the spectrum pattern is discovered in it. This model provides two dimensional (retention time and wavelength) fingerprints for pigment characterization which is proven to be more accurate than one dimensional fingerprint (fixed wavelength). Moreover, by mimicking interconnection of the neuron in the nervous systems of the human brain, the model have learning ability that could be replacing expert judgement on evaluating spectrum pattern. In the preprocessing step, principal component analysis (PCA) was used to reduce the huge dimension of the chromatographic data. The aim of this step is to simplify the model and accelerate the identification process. Six photosynthetic pigments i.e. zeaxantin, pheophytin a, α-carotene, β-carotene, lycopene and lutein could be well identified by the model with accuracy up to 85.33% and processing time less than 1 second.

Standardization of the Descemet membrane endothelial keratoplasty technique: Outcomes of the first 450 consecutive cases.

Science.gov (United States)

Satué, M; Rodríguez-Calvo-de-Mora, M; Naveiras, M; Cabrerizo, J; Dapena, I; Melles, G R J

2015-08-01

To evaluate the clinical outcome of the first 450 consecutive cases after Descemet membrane endothelial keratoplasty (DMEK), as well as the effect of standardization of the technique. Comparison between 3 groups: Group I: (cases 1-125), as the extended learning curve; Group II: (cases 126-250), transition to technique standardization; Group III: (cases 251-450), surgery with standardized technique. Best corrected visual acuity, endothelial cell density, pachymetry and intra- and postoperative complications were evaluated before, and 1, 3 and 6 months after DMEK. At 6 months after surgery, 79% of eyes reached a best corrected visual acuity of≥0.8 and 43%≥1.0. Mean preoperative endothelial cell density was 2,530±220 cells/mm2 and 1,613±495 at 6 months after surgery. Mean pachymetry measured 668±92 μm and 526±46 μm pre- and (6 months) postoperatively, respectively. There were no significant differences in best corrected visual acuity, endothelial cell density and pachymetry between the 3 groups (P > .05). Graft detachment presented in 17.3% of the eyes. The detachment rate declined from 24% to 12%, and the rate of secondary surgeries from 9.6% to 3.5%, from group I to III respectively. Visual outcomes and endothelial cell density after DMEK are independent of the technique standardization. However, technique standardization may have contributed to a lower graft detachment rate and a relatively low number of secondary interventions required. As such, DMEK may become the first choice of treatment in corneal endothelial disease. Copyright © 2014 Sociedad Española de Oftalmología. Published by Elsevier España, S.L.U. All rights reserved.

Exploration and classification of chromatographic fingerprints as additional tool for identification and quality control of several Artemisia species.

Science.gov (United States)

Alaerts, Goedele; Pieters, Sigrid; Logie, Hans; Van Erps, Jürgen; Merino-Arévalo, Maria; Dejaegher, Bieke; Smeyers-Verbeke, Johanna; Vander Heyden, Yvan

2014-07-01

-analysis technique. Samples of different quality could be indicated on the score plots. No multi-component analysis was required to reach the goal. Furthermore, differences related to the origin of some of the not-certified samples were shown. The importance of the specific herbal part used for its identification was also presented. In addition, no differences were observed among fingerprints of lyophilised or conditioned-air dried samples. Finally, a classification technique, Soft Independent Modelling by Class Analogy (SIMCA), was successfully evaluated as identification technique for unknown samples. Six additional Artemisia species (29 herbal samples) were identified as not belonging to any of the four modelled classes. The developed chromatographic fingerprints and the evaluation of the entire profiles provide an added value to the distinction, identification and quality control of the simultaneously investigated Artemisia species. Copyright © 2014 Elsevier B.V. All rights reserved.

Paper chromatographic behavior of tetranitronitrosylruthenate and its decomposition products

International Nuclear Information System (INIS)

Akatsu, Eiko

1981-01-01

The paper chromatographic behavior of tetranitronitrosylruthenate was examined together with its decomposition products. First, Rf values at various eluting conditions were studied with five kinds of papers, since there was a discrepancy among the reported Rf values. Usually Rf of 0.9 was obtained by the recommended procedure of Wain, et al. Second, stability of the tetranitrosylruthenate in water was followed by paper chromatography. No change was found until 200 days passed. Third, the tetranitronitrosylruthenate was warmed in acid, and its decomposition products were studied through the paper chromatography. The paper chromatographic behavior showed that the sample kept in water more than 200 days seemed to contain a dinitro complex, and the sample warmed in acid seemed to be decomposed to a mononitro complex of further. (author)

Manual of Standard Operating Procedures for Veterinary Drug Residue Analysis

International Nuclear Information System (INIS)

2016-01-01

Laboratories are crucial to national veterinary drug residue monitoring programmes. However, one of the main challenges laboratories encounter is obtaining access to relevant methods of analysis. Thus, in addition to training, providing technical advice and transferring technology, the Joint FAO/IAEA Division of Nuclear Techniques in Food and Agriculture has resolved to develop clear and practical manuals to support Member State laboratories. The Coordinated Research Project (CRP) on Development of Radiometric and Allied Analytical Methods to Strengthen Residue Control Programs for Antibiotic and Anthelmintic Veterinary Drug Residues has developed a number of analytical methods as standard operating procedures (SOPs), which are now compiled here. This publication contains SOPs on chromatographic and spectrometric techniques, as well as radioimmunoassay and associated screening techniques, for various anthelmintic and antimicrobial veterinary drug residue analysis. Some analytical method validation protocols are also included. The publication is primarily aimed at food and environmental safety laboratories involved in testing veterinary drug residues, including under organized national residue monitoring programmes. It is expected to enhance laboratory capacity building and competence through the use of radiometric and complementary tools and techniques. The publication is also relevant for applied research on residues of veterinary drugs in food and environmental samples

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

Energy Technology Data Exchange (ETDEWEB)

Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

2005-02-15

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

International Nuclear Information System (INIS)

Pyo, Dong Jin; Lim, Chang Hyun

2005-01-01

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

Micro-column plasma emission liquid chromatograph. [Patent application

Science.gov (United States)

Gay, D.D.

1982-08-12

In a direct current plasma emission spectrometer for use in combination with a microcolumn liquid chromatograph, an improved plasma source unit is claimed. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

Dimethylthioarsinic anhydride: A standard for arsenic speciation

Energy Technology Data Exchange (ETDEWEB)

Fricke, Michael [United States Environmental Protection Agency, National Exposure Research Laboratory, Microbiological and Chemical Exposure Assessment Research Division, 26 W. Martin Luther King Drive, Cincinnati, OH 45268 (United States); Zeller, Matthias [STaRBURSTT-Cyberdiffraction Consortium, Department of Chemistry, Youngstown State University, One University Plaza, Youngstown, OH 44555-3663 (United States); Cullen, William [Department of Chemistry, University of British Columbia, 2036 Main Mall, Vancouver, BC, V6T 1Z1 (Canada); Witkowski, Mark [Food and Drug Administration, Forensic Chemistry Center, Vibrational Spectroscopy Laboratory, 6751 Steger Drive, Cincinnati, OH 45237 (United States); Creed, John [United States Environmental Protection Agency, National Exposure Research Laboratory, Microbiological and Chemical Exposure Assessment Research Division, 26 W. Martin Luther King Drive, Cincinnati, OH 45268 (United States)]. E-mail: creed.jack@epa.gov

2007-01-30

Dimethylthioarsinic acid (DMTA{sup V}) has recently been identified in biological, dietary and environmental matrices. The relevance of this compound to the toxicity of arsenic in humans is unknown and further exposure assessment and metabolic studies are difficult to conduct because of the unavailability of a well characterized standard. The synthesis of DMTA{sup V} was accomplished by the reaction of dimethylarsinic acid (DMA{sup V}) with hydrogen sulfide. The initial reaction product produced is DMTA{sup V} but multiple products over the course of the reaction are also observed. Therefore, a chromatographic separation was developed to monitor the reaction progress via LC-ICP-MS. In this synthesis, conversion of DMA{sup V} to DMTA{sup V} was not taken to completion to avoid the production of side products. The product was isolated from the starting material by standard organic techniques. Single crystal diffraction demonstrated that solid DMTA{sup V} is present in the form of the oxygen-bridged dimethylthioarsinic anhydride. Dissolution of the anhydride in water produces the acid form of DMTA{sup V} and the aqueous phase DMTA{sup V} provided a characteristic molecular ion of m/z 155 by LC-ESI-MS. The synthesis and isolation of dimethylthioarsinic anhydride provides a stable crystalline standard suitable for identification, toxicological study and exposure assessment of dimethylthioarsinic acid.

Liquid chromatographic-tandem mass spectrometric assay for ...

African Journals Online (AJOL)

Methods: Blood and urine samples were obtained from healthy volunteers who admitted to not being on any medications. The investigated analytes were chromatographically separated on a C18 column (Luna®-PFP 100Å column, 50 mm × 2.0 mm i.d., 3.0 μm) with the aid of a mobile phase containing A; acetonitrile (ACN) ...

Contribution to the standardization of the chromatographic conditions for the lipophilicity assessment of neutral and basic drugs

Energy Technology Data Exchange (ETDEWEB)

Giaginis, Costas [Department of Pharmaceutical Chemistry, School of Pharmacy, University of Athens, Panepistimiopolis, Zografou, Athens 15771 (Greece); Department of Forensic Medicine and Toxicology, Medical School, University of Athens, 75 Mikras Asias Street, Athens 11527 (Greece); Theocharis, Stamatios [Department of Forensic Medicine and Toxicology, Medical School, University of Athens, 75 Mikras Asias Street, Athens 11527 (Greece); Tsantili-Kakoulidou, Anna [Department of Pharmaceutical Chemistry, School of Pharmacy, University of Athens, Panepistimiopolis, Zografou, Athens 15771 (Greece)]. E-mail: tsantili@pharm.uoa.gr

2006-07-28

The chromatographic conditions aiming to a better simulation of n-octanol-water partitioning using a base deactivated silica (BDS) column as stationary phase were investigated for structurally diverse basic and neutral drugs. Extrapolated retention factors log k{sub w}, determined using different methanol fractions as organic modifier, were considered as lipophilicity indices. The effect of n-decylamine and n-octanol as mobile phase additives was examined and the appropriateness of the final retention outcome to reproduce lipophilicity data was evaluated. Moreover, the influence of n-octanol on the linearity of the log k/methanol fraction relationship and on the uniformity of the retention mechanism was investigated. 1:1 correlation between log k{sub w} values and the logarithm of the distribution coefficient (log D) was established for basic drugs in presence of both n-decylamine and n-octanol as mobile phase additives. However, for neutral drugs n-decylamine proved to be a sufficient and more important factor than n-octanol.

Contribution to the standardization of the chromatographic conditions for the lipophilicity assessment of neutral and basic drugs

International Nuclear Information System (INIS)

Giaginis, Costas; Theocharis, Stamatios; Tsantili-Kakoulidou, Anna

2006-01-01

The chromatographic conditions aiming to a better simulation of n-octanol-water partitioning using a base deactivated silica (BDS) column as stationary phase were investigated for structurally diverse basic and neutral drugs. Extrapolated retention factors log k w , determined using different methanol fractions as organic modifier, were considered as lipophilicity indices. The effect of n-decylamine and n-octanol as mobile phase additives was examined and the appropriateness of the final retention outcome to reproduce lipophilicity data was evaluated. Moreover, the influence of n-octanol on the linearity of the log k/methanol fraction relationship and on the uniformity of the retention mechanism was investigated. 1:1 correlation between log k w values and the logarithm of the distribution coefficient (log D) was established for basic drugs in presence of both n-decylamine and n-octanol as mobile phase additives. However, for neutral drugs n-decylamine proved to be a sufficient and more important factor than n-octanol

Development and Validation of a Liquid Chromatographic Method ...

African Journals Online (AJOL)

A liquid chromatographic method for the simultaneous determination of six human immunodeficiency virus (HIV) protease inhibitors, indinavir, saquinavir, ritonavir, amprenavir, nelfinavir and lopinavir, was developed and validated. Optimal separation was achieved on a PLRP-S 100 Å, 250 x 4.6 mm I.D. column maintained ...

Sensitive high performance liquid chromatographic method for the ...

African Journals Online (AJOL)

A new simple, sensitive, cost-effective and reproducible high performance liquid chromatographic (HPLC) method for the determination of proguanil (PG) and its metabolites, cycloguanil (CG) and 4-chlorophenylbiguanide (4-CPB) in urine and plasma is described. The extraction procedure is a simple three-step process ...

Studies on Brucella interferon: Chromatographic behaviour and purification

International Nuclear Information System (INIS)

Bousquet-Ucla, C.; Wietzerbin, J.; Falcoff, E.

1980-01-01

Interferon was induced by infecting mice with Brucella suis. Serum containing interferon activity was analyzed by chromatography on Concanavalin A-Sepharose and Phenyl-Sepharose CL-4B columns. Antiviral activity was completely retained by the lectin column indicating that all the interferon molecules are glycosylated. The chromatographic behaviour of Brucella interferon on Phenyl-Sepharose CL-4B show that, like other interferons, Brucella interferon displays hydrophobic properties. However, the hydrophobicity of the interferon molecule was masked in the crude preparation and was only detectable when purified Brucella interferon was used for chromatography. The antigenic properties of Brucella interferon provided the means for developing an affinity chromatographic method resulting in about 60.000 fold purification. As in the case of viral interferon, treatment of L cells with Brucella interferon induced specific enhanced in vitro phosphorylation of a 67.000 molecular weight protein after incubation of cell extracts with doublestranded RNA and [γ- 32 p]ATP. (auth.)

Molecular Weights of Bovine and Porcine Heparin Samples: Comparison of Chromatographic Methods and Results of a Collaborative Survey

Directory of Open Access Journals (Sweden)

Sabrina Bertini

2017-07-01

Full Text Available In a collaborative study involving six laboratories in the USA, Europe, and India the molecular weight distributions of a panel of heparin sodium samples were determined, in order to compare heparin sodium of bovine intestinal origin with that of bovine lung and porcine intestinal origin. Porcine samples met the current criteria as laid out in the USP Heparin Sodium monograph. Bovine lung heparin samples had consistently lower average molecular weights. Bovine intestinal heparin was variable in molecular weight; some samples fell below the USP limits, some fell within these limits and others fell above the upper limits. These data will inform the establishment of pharmacopeial acceptance criteria for heparin sodium derived from bovine intestinal mucosa. The method for MW determination as described in the USP monograph uses a single, broad standard calibrant to characterize the chromatographic profile of heparin sodium on high-resolution silica-based GPC columns. These columns may be short-lived in some laboratories. Using the panel of samples described above, methods based on the use of robust polymer-based columns have been developed. In addition to the use of the USP’s broad standard calibrant for heparin sodium with these columns, a set of conditions have been devised that allow light-scattering detected molecular weight characterization of heparin sodium, giving results that agree well with the monograph method. These findings may facilitate the validation of variant chromatographic methods with some practical advantages over the USP monograph method.

Molecular Weights of Bovine and Porcine Heparin Samples: Comparison of Chromatographic Methods and Results of a Collaborative Survey.

Science.gov (United States)

Bertini, Sabrina; Risi, Giulia; Guerrini, Marco; Carrick, Kevin; Szajek, Anita Y; Mulloy, Barbara

2017-07-19

In a collaborative study involving six laboratories in the USA, Europe, and India the molecular weight distributions of a panel of heparin sodium samples were determined, in order to compare heparin sodium of bovine intestinal origin with that of bovine lung and porcine intestinal origin. Porcine samples met the current criteria as laid out in the USP Heparin Sodium monograph. Bovine lung heparin samples had consistently lower average molecular weights. Bovine intestinal heparin was variable in molecular weight; some samples fell below the USP limits, some fell within these limits and others fell above the upper limits. These data will inform the establishment of pharmacopeial acceptance criteria for heparin sodium derived from bovine intestinal mucosa. The method for MW determination as described in the USP monograph uses a single, broad standard calibrant to characterize the chromatographic profile of heparin sodium on high-resolution silica-based GPC columns. These columns may be short-lived in some laboratories. Using the panel of samples described above, methods based on the use of robust polymer-based columns have been developed. In addition to the use of the USP's broad standard calibrant for heparin sodium with these columns, a set of conditions have been devised that allow light-scattering detected molecular weight characterization of heparin sodium, giving results that agree well with the monograph method. These findings may facilitate the validation of variant chromatographic methods with some practical advantages over the USP monograph method.

Critical evaluation of sample pretreatment techniques.

Science.gov (United States)

Hyötyläinen, Tuulia

2009-06-01

Sample preparation before chromatographic separation is the most time-consuming and error-prone part of the analytical procedure. Therefore, selecting and optimizing an appropriate sample preparation scheme is a key factor in the final success of the analysis, and the judicious choice of an appropriate procedure greatly influences the reliability and accuracy of a given analysis. The main objective of this review is to critically evaluate the applicability, disadvantages, and advantages of various sample preparation techniques. Particular emphasis is placed on extraction techniques suitable for both liquid and solid samples.

Modification of the cranial closing wedge ostectomy technique for the treatment of canine cruciate disease. Description and comparison with standard technique.

Science.gov (United States)

Wallace, A M; Addison, E S; Smith, B A; Radke, H; Hobbs, S J

2011-01-01

To describe a modification of the cranial closing wedge ostectomy (CCWO) technique and to compare its efficacy to the standard technique on cadaveric specimens. The standard and modified CCWO technique were applied to eight pairs of cadaveric tibiae. The following parameters were compared following the ostectomy: degrees of plateau levelling achieved (degrees), tibial long axis shift (degrees), reduction in tibial length (mm), area of bone wedge removed (cm²), and the area of proximal fragment (cm²). The size of the removed wedge of bone and the reduction in tibial length were significantly less with the modified CCWO technique. The modified CCWO has two main advantages. Firstly a smaller wedge is removed, allowing a greater preservation of bone stock in the proximal tibia, which is advantageous for implant placement. Secondly, the tibia is shortened to a lesser degree, which might reduce the risk of recurvatum, fibular fracture and patella desmitis. These factors are particularly propitious for the application of this technique to Terrier breeds with excessive tibial plateau angle, where large angular corrections are required. The modified CCWO is equally effective for plateau levelling and results in an equivalent tibial long-axis shift. A disadvantage with the modified technique is that not all of the cross sectional area of the distal fragment contributes to load sharing at the osteotomy.

[Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter].

Science.gov (United States)

Hao, Liang; Wu, Dapeng; Guan, Yafeng

2014-09-01

The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

Preparation and evaluation of 99mTc-cefuroxime, a potential infection specific imaging agent: A reliable thin layer chromatographic system to delineate impurities from the 99mTc-antibiotic

International Nuclear Information System (INIS)

Chattopadhyay, Sankha; Ghosh, Mayuri; Sett, Sucharita; Das, Malay Kanti; Chandra, Susmita; De, Kakali; Mishra, Mridula; Sinha, Samarendu; Ranjan Sarkar, Bharat; Ganguly, Shantanu

2012-01-01

Technetium-99m labelled cefuroxime, a second-generation cephalosporin antibiotic and potential bacteria specific infection imaging agent was evaluated. A good radiochemical purity (95%) of the labelled product was obtained after filtering the reaction mixture through a 0.22 μm filter. Scintigraphy study of the purified product showed uptake in infectious lesions 45 min after injection and abscess-to-muscle ratios were found to be 1.80, 1.85 and 1.88 at 45 min, 1.5 hr and 3 hr, respectively. A versatile and reliable chromatographic technique to assess the radiochemical purity of 99m Tc-cefuroxime has also been described. - Highlights: ► Preparation of 99m Tc-cefuroxime in presence of Sn-tartrate as reducing agent. ► Physiochemical and biological evaluation of 99m Tc-cefuroxime. ► A versatile and reliable chromatographic technique to assess the radiochemical purity of 99m Tc-cefuroxime.

Assessment of Snared-Loop Technique When Standard Retrieval of Inferior Vena Cava Filters Fails

International Nuclear Information System (INIS)

Doody, Orla; Noe, Geertje; Given, Mark F.; Foley, Peter T.; Lyon, Stuart M.

2009-01-01

Purpose To identify the success and complications related to a variant technique used to retrieve inferior vena cava filters when simple snare approach has failed. Methods A retrospective review of all Cook Guenther Tulip filters and Cook Celect filters retrieved between July 2006 and February 2008 was performed. During this period, 130 filter retrievals were attempted. In 33 cases, the standard retrieval technique failed. Retrieval was subsequently attempted with our modified retrieval technique. Results The retrieval was successful in 23 cases (mean dwell time, 171.84 days; range, 5-505 days) and unsuccessful in 10 cases (mean dwell time, 162.2 days; range, 94-360 days). Our filter retrievability rates increased from 74.6% with the standard retrieval method to 92.3% when the snared-loop technique was used. Unsuccessful retrieval was due to significant endothelialization (n = 9) and caval penetration by the filter (n = 1). A single complication occurred in the group, in a patient developing pulmonary emboli after attempted retrieval. Conclusion The technique we describe increased the retrievability of the two filters studied. Hook endothelialization is the main factor resulting in failed retrieval and continues to be a limitation with these filters.

Liquid-chromatographic determination of sarafloxacin residues in channel catfish muscle-tissue

Science.gov (United States)

Meinertz, J.R.; Dawson, V.K.; Gingerich, W.H.; Cheng, B.; Tubergen, M.M.

1994-01-01

A liquid chromatographic method is described for the determination of sarafloxacin hydrochloride residues i n channel catfish (ictalurus punctatus) fillets. Sarafloxacin was extracted from fillet tissue with acetonitrile=water (1 + 1). The extract was centrifuged and the supernatant was partitioned with hexane. The aqueous fraction was filtered through a 0.45 Mum filter and evaporated to dryness. The sample was redissolved with 20% acetonitrile-methanol (3 + 2) and 80% trifluoroacetic acid (0.1%), Centrifuged, and filtered to remove proteins. Samples were analyzed by chromatography with gradient elution on a c18 column and with fluorescence detection (excitation at 280 nm and emission above 389 nm). Mean recoveries ranged from 85.4 To 104%, and relative standard deviations ranged from 1.06 To 5.58% In samples spiked at concentrations of 10.0-863.8 Ng/g. The method detection limit for sarafloxacin was 1.4 Ng/g.

[Application of robustness test for assessment of the measurement uncertainty at the end of development phase of a chromatographic method for quantification of water-soluble vitamins].

Science.gov (United States)

Ihssane, B; Bouchafra, H; El Karbane, M; Azougagh, M; Saffaj, T

2016-05-01

We propose in this work an efficient way to evaluate the measurement of uncertainty at the end of the development step of an analytical method, since this assessment provides an indication of the performance of the optimization process. The estimation of the uncertainty is done through a robustness test by applying a Placquett-Burman design, investigating six parameters influencing the simultaneous chromatographic assay of five water-soluble vitamins. The estimated effects of the variation of each parameter are translated into standard uncertainty value at each concentration level. The values obtained of the relative uncertainty do not exceed the acceptance limit of 5%, showing that the procedure development was well done. In addition, a statistical comparison conducted to compare standard uncertainty after the development stage and those of the validation step indicates that the estimated uncertainty are equivalent. The results obtained show clearly the performance and capacity of the chromatographic method to simultaneously assay the five vitamins and suitability for use in routine application. Copyright © 2015 Académie Nationale de Pharmacie. Published by Elsevier Masson SAS. All rights reserved.

Separation and determination of high-carbon alcohols using method of column chromatographic and gas-chromatographic analysis

International Nuclear Information System (INIS)

Kang Zhongrong; Li Biping; Zeng Yongchang

1988-01-01

This paper describes the separation and determination of high-carbon alcohols from amine extractant by using the method of column chromatography of aluminium oxide and gas-chromatographic analysis. The total conent of high-carbon alcohols is determined by the method of column chromatography, while the components of the high-carbon alcohols and their relative contents are determined by the method of gas-chromatography. A simple reliable and practical method is provided for the analysis of high-carbon alcohol from the amine extractant in this paper

Vibrational Spectroscopy of Chromatographic Interfaces

Energy Technology Data Exchange (ETDEWEB)

Jeanne E. Pemberton

2011-03-10

Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

Comparison of anthropometry with photogrammetry based on a standardized clinical photographic technique using a cephalostat and chair.

Science.gov (United States)

Han, Kihwan; Kwon, Hyuk Joon; Choi, Tae Hyun; Kim, Jun Hyung; Son, Daegu

2010-03-01

The aim of this study was to standardize clinical photogrammetric techniques, and to compare anthropometry with photogrammetry. To standardize clinical photography, we have developed a photographic cephalostat and chair. We investigated the repeatability of the standardized clinical photogrammetric technique. Then, with 40 landmarks, a total of 96 anthropometric measurement items was obtained from 100 Koreans. Ninety six photogrammetric measurements from the same subjects were also obtained from standardized clinical photographs using Adobe Photoshop version 7.0 (Adobe Systems Corporation, San Jose, CA, USA). The photogrammetric and anthropometric measurement data (mm, degree) were then compared. A coefficient was obtained by dividing the anthropometric measurements by the photogrammetric measurements. The repeatability of the standardized photography was statistically significantly high (p=0.463). Among the 96 measurement items, 44 items were reliable; for these items the photogrammetric measurements were not different to the anthropometric measurements. The remaining 52 items must be classified as unreliable. By developing a photographic cephalostat and chair, we have standardized clinical photogrammetric techniques. The reliable set of measurement items can be used as anthropometric measurements. For unreliable measurement items, applying a suitable coefficient to the photogrammetric measurement allows the anthropometric measurement to be obtained indirectly.

UPLC-ICP-MS - a fast technique for speciation analysis

DEFF Research Database (Denmark)

Bendahl, L.; Sturup, S.; Gammelgaard, Bente

2005-01-01

aqueous selenium standards were separated within 1.2 min on a 1.00 id x 50 mm reversed phase column in an ion-pair chromatographic system using a flow rate of 200 mu L min(-1). Hence, analysis times could be reduced to 1/10 compared with ordinary HPLC for aqueous standards. The precision and detection...... the use of short columns. Hence, analysis times could be halved without loss of separation efficiency in this biological sample...

Evaluation of a gas chromatograph with a novel surface acoustic wave detector (SAW GC) for screening of volatile organic compounds in Hanford waste tank samples

International Nuclear Information System (INIS)

Lockrem, L.L.

1998-01-01

A novel instrument, a gas chromatograph with a Surface Acoustic Wave Detector (SAW GC), was evaluated for the screening of organic compounds in Hanford tank headspace vapors. Calibration data were developed for the most common organic compounds, and the accuracy and precision were measured with a certified standard. The instrument was tested with headspace samples collected from seven Hanford waste tanks

Manual of Standard Operating Procedures for Veterinary Drug Residue Analysis (Spanish Edition)

International Nuclear Information System (INIS)

2017-01-01

Laboratories are crucial to national veterinary drug residue monitoring programmes. However, one of the main challenges laboratories encounter is obtaining access to relevant methods of analysis. Thus, in addition to training, providing technical advice and transferring technology, the Joint FAO/IAEA Division of Nuclear Techniques in Food and Agriculture has resolved to develop clear and practical manuals to support Member State laboratories. The Coordinated Research Project (CRP) on Development of Radiometric and Allied Analytical Methods to Strengthen Residue Control Programs for Antibiotic and Anthelmintic Veterinary Drug Residues has developed a number of analytical methods as standard operating procedures (SOPs), which are now compiled here. This publication contains SOPs on chromatographic and spectrometric techniques, as well as radioimmunoassay and associated screening techniques, for various anthelmintic and antimicrobial veterinary drug residue analysis. Some analytical method validation protocols are also included. The publication is primarily aimed at food and environmental safety laboratories involved in testing veterinary drug residues, including under organized national residue monitoring programmes. It is expected to enhance laboratory capacity building and competence through the use of radiometric and complementary tools and techniques. The publication is also relevant for applied research on residues of veterinary drugs in food and environmental samples

Manual of Standard Operating Procedures for Veterinary Drug Residue Analysis (French Edition)

International Nuclear Information System (INIS)

2017-01-01

Laboratories are crucial to national veterinary drug residue monitoring programmes. However, one of the main challenges laboratories encounter is obtaining access to relevant methods of analysis. Thus, in addition to training, providing technical advice and transferring technology, the Joint FAO/IAEA Division of Nuclear Techniques in Food and Agriculture has resolved to develop clear and practical manuals to support Member State laboratories. The Coordinated Research Project (CRP) on Development of Radiometric and Allied Analytical Methods to Strengthen Residue Control Programs for Antibiotic and Anthelmintic Veterinary Drug Residues has developed a number of analytical methods as standard operating procedures (SOPs), which are now compiled here. This publication contains SOPs on chromatographic and spectrometric techniques, as well as radioimmunoassay and associated screening techniques, for various anthelmintic and antimicrobial veterinary drug residue analysis. Some analytical method validation protocols are also included. The publication is primarily aimed at food and environmental safety laboratories involved in testing veterinary drug residues, including under organized national residue monitoring programmes. It is expected to enhance laboratory capacity building and competence through the use of radiometric and complementary tools and techniques. The publication is also relevant for applied research on residues of veterinary drugs in food and environmental samples

Similarity analyses of chromatographic herbal fingerprints: a review.

Science.gov (United States)

Goodarzi, Mohammad; Russell, Paul J; Vander Heyden, Yvan

2013-12-04

Herbal medicines are becoming again more popular in the developed countries because being "natural" and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order to help determining substantial equivalence using fingerprint approaches, a quantitative measurement of similarity is required. In this paper, different (dis)similarity approaches, such as (dis)similarity metrics or exploratory analysis approaches applied on herbal medicinal fingerprints, are discussed and illustrated with several case studies. Copyright © 2013

Chromatographic fingerprint similarity analysis for pollutant source identification

International Nuclear Information System (INIS)

Xie, Juan-Ping; Ni, Hong-Gang

2015-01-01

In the present study, a similarity analysis method was proposed to evaluate the source-sink relationships among environmental media for polybrominated diphenyl ethers (PBDEs), which were taken as the representative contaminants. Chromatographic fingerprint analysis has been widely used in the fields of natural products chemistry and forensic chemistry, but its application to environmental science has been limited. We established a library of various sources of media containing contaminants (e.g., plastics), recognizing that the establishment of a more comprehensive library allows for a better understanding of the sources of contamination. We then compared an environmental complex mixture (e.g., sediment, soil) with the profiles in the library. These comparisons could be used as the first step in source tracking. The cosine similarities between plastic and soil or sediment ranged from 0.53 to 0.68, suggesting that plastic in electronic waste is an important source of PBDEs in the environment, but it is not the only source. A similarity analysis between soil and sediment indicated that they have a source-sink relationship. Generally, the similarity analysis method can encompass more relevant information of complex mixtures in the environment than a profile-based approach that only focuses on target pollutants. There is an inherent advantage to creating a data matrix containing all peaks and their relative levels after matching the peaks based on retention times and peak areas. This data matrix can be used for source identification via a similarity analysis without quantitative or qualitative analysis of all chemicals in a sample. - Highlights: • Chromatographic fingerprint analysis can be used as the first step in source tracking. • Similarity analysis method can encompass more relevant information of pollution. • The fingerprints strongly depend on the chromatographic conditions. • A more effective and robust method for identifying similarities is required

A no-gold-standard technique for objective assessment of quantitative nuclear-medicine imaging methods.

Science.gov (United States)

Jha, Abhinav K; Caffo, Brian; Frey, Eric C

2016-04-07

The objective optimization and evaluation of nuclear-medicine quantitative imaging methods using patient data is highly desirable but often hindered by the lack of a gold standard. Previously, a regression-without-truth (RWT) approach has been proposed for evaluating quantitative imaging methods in the absence of a gold standard, but this approach implicitly assumes that bounds on the distribution of true values are known. Several quantitative imaging methods in nuclear-medicine imaging measure parameters where these bounds are not known, such as the activity concentration in an organ or the volume of a tumor. We extended upon the RWT approach to develop a no-gold-standard (NGS) technique for objectively evaluating such quantitative nuclear-medicine imaging methods with patient data in the absence of any ground truth. Using the parameters estimated with the NGS technique, a figure of merit, the noise-to-slope ratio (NSR), can be computed, which can rank the methods on the basis of precision. An issue with NGS evaluation techniques is the requirement of a large number of patient studies. To reduce this requirement, the proposed method explored the use of multiple quantitative measurements from the same patient, such as the activity concentration values from different organs in the same patient. The proposed technique was evaluated using rigorous numerical experiments and using data from realistic simulation studies. The numerical experiments demonstrated that the NSR was estimated accurately using the proposed NGS technique when the bounds on the distribution of true values were not precisely known, thus serving as a very reliable metric for ranking the methods on the basis of precision. In the realistic simulation study, the NGS technique was used to rank reconstruction methods for quantitative single-photon emission computed tomography (SPECT) based on their performance on the task of estimating the mean activity concentration within a known volume of interest

A no-gold-standard technique for objective assessment of quantitative nuclear-medicine imaging methods

International Nuclear Information System (INIS)

Jha, Abhinav K; Frey, Eric C; Caffo, Brian

2016-01-01

The objective optimization and evaluation of nuclear-medicine quantitative imaging methods using patient data is highly desirable but often hindered by the lack of a gold standard. Previously, a regression-without-truth (RWT) approach has been proposed for evaluating quantitative imaging methods in the absence of a gold standard, but this approach implicitly assumes that bounds on the distribution of true values are known. Several quantitative imaging methods in nuclear-medicine imaging measure parameters where these bounds are not known, such as the activity concentration in an organ or the volume of a tumor. We extended upon the RWT approach to develop a no-gold-standard (NGS) technique for objectively evaluating such quantitative nuclear-medicine imaging methods with patient data in the absence of any ground truth. Using the parameters estimated with the NGS technique, a figure of merit, the noise-to-slope ratio (NSR), can be computed, which can rank the methods on the basis of precision. An issue with NGS evaluation techniques is the requirement of a large number of patient studies. To reduce this requirement, the proposed method explored the use of multiple quantitative measurements from the same patient, such as the activity concentration values from different organs in the same patient. The proposed technique was evaluated using rigorous numerical experiments and using data from realistic simulation studies. The numerical experiments demonstrated that the NSR was estimated accurately using the proposed NGS technique when the bounds on the distribution of true values were not precisely known, thus serving as a very reliable metric for ranking the methods on the basis of precision. In the realistic simulation study, the NGS technique was used to rank reconstruction methods for quantitative single-photon emission computed tomography (SPECT) based on their performance on the task of estimating the mean activity concentration within a known volume of interest

Assessment of the chromatographic lipophilicity of eight cephalosporins on different stationary phases.

Science.gov (United States)

Dąbrowska, Monika; Starek, Małgorzata; Komsta, Łukasz; Szafrański, Przemysław; Stasiewicz-Urban, Anna; Opoka, Włodzimierz

2017-04-01

The retention behaviors were investigated for a series of eight cephalosporins in thin-layer chromatography (TLC) using stationary phases of RP-2, RP-8, RP-18, NH 2 , DIOL, and CN chemically bonded silica gel. Additionally, various binary mobile phases (water/methanol and water/acetone) were used in different volume proportions. The retention behavior of the analyzed molecules was defined by R M0 constant. In addition, reversed phase high performance liquid chromatography (RP-HPLC) was performed in lipophilicity studies by using immobilized artificial membrane (IAM) stationary phase. Obtained chromatographic data (R M0 and logk' IAM ) were correlated with the lipophilicity, expressed as values of the log calculated (logP calc ) and experimental (logP exp(shake-flask) ) partition coefficient. Principal component analysis (PCA) was applied in order to obtain an overview of similarity or dissimilarity among the analyzed compounds. Hierarchical cluster analysis (HCA) was performed to compare the separation characteristics of the applied stationary phases. This study was undertaken to identify the best chromatographic system and chromatographic data processing method to enable the prediction of logP values. A comprehensive chromatographic investigation into the retention of the analyzed cephalosporins revealed a similar behavior on RP-18, RP-8 and CN stationary phases. The weak correlations obtained between experimental and certain computed lipophilicity indices revealed that R M0 and PC1/RM are relevant lipophilicity parameters and the RP-8, CN and RP-18 plates are appropriate stationary phases for lipophilicity investigation, whereas computational approaches still cannot fully replace experimentation. Copyright © 2017 Elsevier B.V. All rights reserved.

Mass spectrometry. [review of techniques

Science.gov (United States)

Burlingame, A. L.; Kimble, B. J.; Derrick, P. J.

1976-01-01

Advances in mass spectrometry (MS) and its applications over the past decade are reviewed in depth, with annotated literature references. New instrumentation and techniques surveyed include: modulated-beam MS, chromatographic MS on-line computer techniques, digital computer-compatible quadrupole MS, selected ion monitoring (mass fragmentography), and computer-aided management of MS data and interpretation. Areas of application surveyed include: organic MS and electron impact MS, field ionization kinetics, appearance potentials, translational energy release, studies of metastable species, photoionization, calculations of molecular orbitals, chemical kinetics, field desorption MS, high pressure MS, ion cyclotron resonance, biochemistry, medical/clinical chemistry, pharmacology, and environmental chemistry and pollution studies.

QSAR models for prediction of chromatographic behavior of homologous Fab variants.

Science.gov (United States)

Robinson, Julie R; Karkov, Hanne S; Woo, James A; Krogh, Berit O; Cramer, Steven M

2017-06-01

While quantitative structure activity relationship (QSAR) models have been employed successfully for the prediction of small model protein chromatographic behavior, there have been few reports to date on the use of this methodology for larger, more complex proteins. Recently our group generated focused libraries of antibody Fab fragment variants with different combinations of surface hydrophobicities and electrostatic potentials, and demonstrated that the unique selectivities of multimodal resins can be exploited to separate these Fab variants. In this work, results from linear salt gradient experiments with these Fabs were employed to develop QSAR models for six chromatographic systems, including multimodal (Capto MMC, Nuvia cPrime, and two novel ligand prototypes), hydrophobic interaction chromatography (HIC; Capto Phenyl), and cation exchange (CEX; CM Sepharose FF) resins. The models utilized newly developed "local descriptors" to quantify changes around point mutations in the Fab libraries as well as novel cluster descriptors recently introduced by our group. Subsequent rounds of feature selection and linearized machine learning algorithms were used to generate robust, well-validated models with high training set correlations (R 2  > 0.70) that were well suited for predicting elution salt concentrations in the various systems. The developed models then were used to predict the retention of a deamidated Fab and isotype variants, with varying success. The results represent the first successful utilization of QSAR for the prediction of chromatographic behavior of complex proteins such as Fab fragments in multimodal chromatographic systems. The framework presented here can be employed to facilitate process development for the purification of biological products from product-related impurities by in silico screening of resin alternatives. Biotechnol. Bioeng. 2017;114: 1231-1240. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

Arsenic speciation in sulfidic waters: reconciling contradictory spectroscopic and chromatographic evidence.

Science.gov (United States)

Planer-Friedrich, Britta; Suess, Elke; Scheinost, Andreas C; Wallschläger, Dirk

2010-12-15

In recent years, analytical methods have been developed that have demonstrated that soluble arsenic-sulfur species constitute a major fraction of dissolved arsenic in sulfidic waters. However, an intense debate is going on about the exact chemical nature of these compounds, since X-ray absorption spectroscopy (XAS) data generated at higher (mmol/L) concentrations suggest the presence of (oxy)thioarsenites in such waters, while ion chromatographic (IC) and mass spectroscopic data at lower (μmol/L to nmol/L) concentrations indicate the presence of (oxy)thioarsenates. In this contribution, we connect and explain these two apparently different types of results. We show by XAS that thioarsenites are the primary reaction products of arsenite and sulfide in geochemical model experiments in the complete absence of oxygen. However, thioarsenites are extremely unstable toward oxidation, and convert rapidly into thioarsenates when exposed to atmospheric oxygen, e.g., while waiting for analysis on the chromatographic autosampler. This problem can only be eliminated when the entire chromatographic process is conducted inside a glovebox. We also show that thioarsenites are unstable toward sample dilution, which is commonly employed prior to chromatographic analysis when ultrasensitive detectors like ICP-MS are used. This instability has two main reasons: if pH changes during dilution, then equilibria between individual arsenic-sulfur species rearrange rapidly due to their different stability regions within the pH range, and if pH is kept constant during dilution, then this changes the ratio between OH(-) and SH(-) in solution, which in turn shifts the underlying speciation equilibria. This problem is avoided by analyzing samples undiluted. Our studies show that thioarsenites appear as thioarsenates in IC analyses if oxygen is not excluded completely, and as arsenite if samples are diluted in alkaline anoxic medium. This also points out that thioarsenites are necessary

A review on sample preparation and chromatographic determination of acephate and methamidophos in

Directory of Open Access Journals (Sweden)

Vijay Kumar

2015-09-01

Full Text Available Acephate and its metabolite methamidophos are common organophosphorus insecticide used for crop protection. High uses of acephate and methamidophos have induced health issues and environmental pollution. Their undesired presence in the environment is creating ecotoxicology and may harm human health. It is therefore essential to detect the presence of acephate and methamidophos even in trace level. In this review, we have tried to accommodate successful methods of detection of acephate and methamidophos in the different biological media. Their recovery and residue analysis in different media such as vegetables, human and animal tissues have also included. The most common method for their determination is based on chromatographic separation and identification. Among different chromatographic methods, LC and GC coupled with different detectors have used. But, they both need extensive pretreatment and cleanup procedure, before undergoing chromatographic separation and identification. LC coupled with mass spectrometry (LCMS is sometime able to detect acephate and methamidophos in ppm level.

Comparison of QuadrapolarTM radiofrequency lesions produced by standard versus modified technique: an experimental model

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Safakish R

2017-06-01

Full Text Available Ramin Safakish Allevio Pain Management Clinic, Toronto, ON, Canada Abstract: Lower back pain (LBP is a global public health issue and is associated with substantial financial costs and loss of quality of life. Over the years, different literature has provided different statistics regarding the causes of the back pain. The following statistic is the closest estimation regarding our patient population. The sacroiliac (SI joint pain is responsible for LBP in 18%–30% of individuals with LBP. Quadrapolar™ radiofrequency ablation, which involves ablation of the nerves of the SI joint using heat, is a commonly used treatment for SI joint pain. However, the standard Quadrapolar radiofrequency procedure is not always effective at ablating all the sensory nerves that cause the pain in the SI joint. One of the major limitations of the standard Quadrapolar radiofrequency procedure is that it produces small lesions of ~4 mm in diameter. Smaller lesions increase the likelihood of failure to ablate all nociceptive input. In this study, we compare the standard Quadrapolar radiofrequency ablation technique to a modified Quadrapolar ablation technique that has produced improved patient outcomes in our clinic. The methodology of the two techniques are compared. In addition, we compare results from an experimental model comparing the lesion sizes produced by the two techniques. Taken together, the findings from this study suggest that the modified Quadrapolar technique provides longer lasting relief for the back pain that is caused by SI joint dysfunction. A randomized controlled clinical trial is the next step required to quantify the difference in symptom relief and quality of life produced by the two techniques. Keywords: lower back pain, radiofrequency ablation, sacroiliac joint, Quadrapolar radiofrequency ablation

An automated multidimensional preparative gas chromatographic system for isolation and enrichment of trace amounts of xenon from ambient air.

Science.gov (United States)

Larson, Tuula; Östman, Conny; Colmsjö, Anders

2011-04-01

The monitoring of radioactive xenon isotopes is one of the principal methods for the detection of nuclear explosions in order to identify clandestine nuclear testing. In this work, a miniaturized, multiple-oven, six-column, preparative gas chromatograph was constructed in order to isolate trace quantities of radioactive xenon isotopes from ambient air, utilizing nitrogen as the carrier gas. The multidimensional chromatograph comprised preparative stainless steel columns packed with molecular sieves, activated carbon, and synthetic carbon adsorbents (e.g., Anasorb®-747 and Carbosphere®). A combination of purification techniques--ambient adsorption, thermal desorption, back-flushing, thermal focusing, and heart cutting--was selectively optimized to produce a well-defined xenon peak that facilitated reproducible heart cutting and accurate quantification. The chromatographic purification of a sample requires approximately 4 h and provides complete separation of xenon from potentially interfering components (such as water vapor, methane, carbon dioxide, and radon) with recovery and accuracy close to 100%. The preparative enrichment process isolates and concentrates a highly purified xenon gas fraction that is suitable for subsequent ultra-low-level γ-, ß/γ-spectroscopic or high-resolution mass spectrometric measurement (e.g., to monitor the gaseous fission products of nuclear explosions at remote locations). The Xenon Processing Unit is a free-standing, relatively lightweight, and transportable system that can be interfaced to a variety of sampling and detection systems. It has a relatively inexpensive, rugged, and compact modular (19-inch rack) design that provides easy access to all parts for maintenance and has a low power requirement.

Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

Directory of Open Access Journals (Sweden)

Sonia T. Hassib

2011-12-01

Full Text Available Simple, accurate and precise reversed-phase liquid chromatographic (LC and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS and trimethoprim (TMP in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9:acetonitrile:water (25:100:50, v/v/v at a flow rate of 1.6 ml min−1 with UV detection at 210 nm for ERS and 280 nm for TMP. Besides, two spectrophotometric methods were applied after reaction with perchloric acid (12 M which gives a colored product with ERS. Then, the spectral interference between the colored product of ERS and TMP was resolved by either ratio spectra derivative spectrophotometry in the first spectrophotometric method or chemometric techniques, namely classical least-squares (CLS, principal component regression (PCR and partial least-squares regression (PLS in the second spectrophotometric method. The results were statistically compared using one-way analysis of variance (ANOVA. The methods developed were satisfactorily applied to the analysis of the pharmaceutical preparation containing the two drugs and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

Standard Test Method for Determining Thermal Neutron Reaction Rates and Thermal Neutron Fluence Rates by Radioactivation Techniques

CERN Document Server

American Society for Testing and Materials. Philadelphia

2008-01-01

1.1 The purpose of this test method is to define a general procedure for determining an unknown thermal-neutron fluence rate by neutron activation techniques. It is not practicable to describe completely a technique applicable to the large number of experimental situations that require the measurement of a thermal-neutron fluence rate. Therefore, this method is presented so that the user may adapt to his particular situation the fundamental procedures of the following techniques. 1.1.1 Radiometric counting technique using pure cobalt, pure gold, pure indium, cobalt-aluminum, alloy, gold-aluminum alloy, or indium-aluminum alloy. 1.1.2 Standard comparison technique using pure gold, or gold-aluminum alloy, and 1.1.3 Secondary standard comparison techniques using pure indium, indium-aluminum alloy, pure dysprosium, or dysprosium-aluminum alloy. 1.2 The techniques presented are limited to measurements at room temperatures. However, special problems when making thermal-neutron fluence rate measurements in high-...

Parameter selection for peak alignment in chromatographic sample profiling: Objective quality indicators and use of control samples

NARCIS (Netherlands)

Peters, S.; van Velzen, E.; Janssen, H.-G.

2009-01-01

In chromatographic profiling applications, peak alignment is often essential as most chromatographic systems exhibit small peak shifts over time. When using currently available alignment algorithms, there are several parameters that determine the outcome of the alignment process. Selecting the

Determination of solute descriptors by chromatographic methods

International Nuclear Information System (INIS)

Poole, Colin F.; Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K.

2009-01-01

The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

Determination of solute descriptors by chromatographic methods.

Science.gov (United States)

Poole, Colin F; Atapattu, Sanka N; Poole, Salwa K; Bell, Andrea K

2009-10-12

The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

Study of interactions between lanthanides/actinides and humic substances by a steric exclusion chromatographic method

International Nuclear Information System (INIS)

Moulin, V.

1986-01-01

The knowledge of cation-humic matter interactions has a great importance in order to have a better understanding of the contribution of these substances to the possible transport of radioactive elements in the geosphere via groundwaters. The method chosen to study the formation of soluble species between lanthanides/actinides ions and humic acids from different origins is a chromatographic technique of gel filtration. This dynamic equilibrium method is based on the separation of the formed complex and the free cation by the porous packing gel. Different elements have been studied by this method: UO 2 2+ , Eu 3+ , Th 4+ and global interaction constants have been calculated. The application to transuranic elements is undertaken. (orig.)

Steroid radioimmunoassay: contribution of standards to blank values, ch. 4

International Nuclear Information System (INIS)

Froelich, M.; Termorshuizen, W.; Kenter, E.; Molenaar, A.J.

1977-01-01

The sensitivity of the radioimmunoassay of steroids is considerably reduced by high blank values which may be derived in part from co-chromatographed standards. Blank levels approach the detection limit of the radioimmunoassay of aldosterone, testosterone and androstenedione when 10,000 dpm (30-35 pg) labelled steroids are used as reference standard. When 20 μg aldosterone, testosterone, or androstenedione is used as standard, blank levels of up to 12,800 pg were measured in the radioimmunoassay. Application of the standards on a separate strip does not improve the results. From the experiments it appeared that contamination took place by transport by the solvent

Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

International Nuclear Information System (INIS)

Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H.

2005-12-01

This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here

Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

Energy Technology Data Exchange (ETDEWEB)

Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

2005-12-15

This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

Science.gov (United States)

Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

2008-01-01

Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

Bioanalytical method transfer considerations of chromatographic-based assays.

Science.gov (United States)

Williard, Clark V

2016-07-01

Bioanalysis is an important part of the modern drug development process. The business practice of outsourcing and transferring bioanalytical methods from laboratory to laboratory has increasingly become a crucial strategy for successful and efficient delivery of therapies to the market. This chapter discusses important considerations when transferring various types of chromatographic-based assays in today's pharmaceutical research and development environment.

Rendezvous technique for recanalization of long-segmental chronic total occlusion above the knee following unsuccessful standard angioplasty.

Science.gov (United States)

Cao, Jun; Lu, Hai-Tao; Wei, Li-Ming; Zhao, Jun-Gong; Zhu, Yue-Qi

2016-04-01

To assess the technical feasibility and efficacy of the rendezvous technique, a type of subintimal retrograde wiring, for the treatment of long-segmental chronic total occlusions above the knee following unsuccessful standard angioplasty. The rendezvous technique was attempted in eight limbs of eight patients with chronic total occlusions above the knee after standard angioplasty failed. The clinical symptoms and ankle-brachial index were compared before and after the procedure. At follow-up, pain relief, wound healing, limb salvage, and the presence of restenosis of the target vessels were evaluated. The rendezvous technique was performed successfully in seven patients (87.5%) and failed in one patient (12.5%). Foot pain improved in all seven patients who underwent successful treatment, with ankle-brachial indexes improving from 0.23 ± 0.13 before to 0.71 ± 0.09 after the procedure (P rendezvous technique is a feasible and effective treatment for chronic total occlusions above the knee when standard angioplasty fails. © The Author(s) 2015.

Chromatographic measurement of hydrogen isotopic and permanent gas impurities in tritium

International Nuclear Information System (INIS)

Warner, D.K.; Kinard, C.; Bohl, D.C.

1976-01-01

This paper describes a gas chromatograph that was designed for dedicated analysis of hydrogen isotopic and permanent gas impurities in tritium and tritium-deuterium mixtures. The instrument that was developed substantially improved the accuracy and precision of hydrogen isotopic analysis in the 20 ppM to one mole percent range as compared with other analytical methods. Several unique design features of the instrument were required due to the radiation and isotopic exchange properties of the tritium in the samples; descriptions of these features are presented along with details of the complete chromatographic system. The experimental procedures used to calibrate the detector and statistically evaluate its performance are given, and the sources of analytical error are cited. The limitations of the present system are also discussed

Elemental analyses of goundwater: demonstrated advantage of low-flow sampling and trace-metal clean techniques over standard techniques

Science.gov (United States)

Creasey, C. L.; Flegal, A. R.

The combined use of both (1) low-flow purging and sampling and (2) trace-metal clean techniques provides more representative measurements of trace-element concentrations in groundwater than results derived with standard techniques. The use of low-flow purging and sampling provides relatively undisturbed groundwater samples that are more representative of in situ conditions, and the use of trace-element clean techniques limits the inadvertent introduction of contaminants during sampling, storage, and analysis. When these techniques are applied, resultant trace-element concentrations are likely to be markedly lower than results based on standard sampling techniques. In a comparison of data derived from contaminated and control groundwater wells at a site in California, USA, trace-element concentrations from this study were 2-1000 times lower than those determined by the conventional techniques used in sampling of the same wells prior to (5months) and subsequent to (1month) the collections for this study. Specifically, the cadmium and chromium concentrations derived using standard sampling techniques exceed the California Maximum Contaminant Levels (MCL), whereas in this investigation concentrations of both of those elements are substantially below their MCLs. Consequently, the combined use of low-flow and trace-metal clean techniques may preclude erroneous reports of trace-element contamination in groundwater. Résumé L'utilisation simultanée de la purge et de l'échantillonnage à faible débit et des techniques sans traces de métaux permet d'obtenir des mesures de concentrations en éléments en traces dans les eaux souterraines plus représentatives que les résultats fournis par les techniques classiques. L'utilisation de la purge et de l'échantillonnage à faible débit donne des échantillons d'eau souterraine relativement peu perturbés qui sont plus représentatifs des conditions in situ, et le recours aux techniques sans éléments en traces limite l

Validação em métodos cromatográficos e eletroforéticos Validation for chromatographic and electrophoretic methods

Directory of Open Access Journals (Sweden)

Marcelo Ribani

2004-10-01

Full Text Available The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the different Brazilian and international regulatory agencies.

Radioisotope Sample Measurement Techniques in Medicine and Biology. Proceedings of the Symposium on Radioisotope Sample Measurement Techniques

International Nuclear Information System (INIS)

1965-01-01

The medical and biological applications of radioisotopes depend on two basically different types of measurements, those on living subjects in vivo and those on samples in vitro. The International Atomic Energy Agency has in the past held several meetings on in vivo measurement techniques, notably whole-body counting and radioisotope scanning. The present volume contains the Proceedings of the first Symposium the Agency has organized to discuss the various aspects of techniques for sample measurement in vitro. The range of these sample measurement techniques is very wide. The sample may weigh a few milligrams or several hundred grams, and may be in the gaseous, liquid or solid state. Its radioactive content may consist of a single, known radioisotope or several unknown ones. The concentration of radioactivity may be low, medium or high. The measurements may be made manually or automatically and any one of the many radiation detectors now available may be used. The 53 papers presented at the Symposium illustrate the great variety of methods now in use for radioactive- sample measurements. The first topic discussed is gamma-ray spectrometry, which finds an increasing number of applications in sample measurements. Other sections of the Proceedings deal with: the use of computers in gamma-ray spectrometry and multiple tracer techniques; recent developments in activation analysis where both gamma-ray spectrometry and computing techniques are applied; thin-layer and paper radio chromatographic techniques for use with low energy beta-ray emitters; various aspects of liquid scintillation counting techniques in the measurement of alpha- and beta-ray emitters, including chemical and colour quenching; autoradiographic techniques; calibration of equipment; and standardization of radioisotopes. Finally, some applications of solid-state detectors are presented; this section may be regarded as a preview of important future developments. The meeting was attended by 203 participants

Post-voiding residual urine and capacity increase in orthotopic urinary diversion: Standard vs modified technique

Directory of Open Access Journals (Sweden)

Bančević Vladimir

2010-01-01

Full Text Available Background/Aim. Ever since the time when the first orthotopic urinary diversion (pouch was performed there has been a constant improvement and modification of surgical techniques. The aim has been to create a urinary reservoir similar to normal bladder, to decrease incidence of postoperative complications and provide an improved life quality. The aim of this study was to compare postvoiding residual urine (PVR and capacity of the pouch constructed by standard or modified technique. Methods. In this prospective and partially retrospective clinical study we included 79 patients. In the group of 41 patients (group ST pouch was constructed using 50-70 cm of the ileum (standard technique. In the group of 38 patients (group MT pouch was constructed using 25-35 cm of the ileum (modified technique. Postoperatively, PVR and pouch capacity were measured using ultrasound in a 3-, 6- and 12-month period. Results. Postoperatively, an increase in PVR and pouch capacity was noticed in both groups. Twelve months postoperatively, PVR was significantly smaller in the group MT than in the group ST [23 (0-90 mL vs 109 (0-570 mL, p < 0,001]. In the same period the pouch capacity was significantly smaller in the MT group than in the ST group [460 (290-710 mL vs 892 (480-2 050 mL, p < 0.001]. Conclusion. Postoperatively, an increase in PVR and pouch capacity was noticed during a 12-month period. A year following the operation the pouch created from a shorter ileal segment reached capacity of the 'normal' bladder with small PVR. The pouch created by standard technique developed an unnecessary large PVR and capacity.

Gas chromatographic analysis of simmondsins and simmondsin ferulates in jojoba meal.

Science.gov (United States)

Van Boven, M; Holser, R; Cokelaere, M; Flo, G; Decuypere, E

2000-09-01

A capillary gas chromatographic method was developed for the simultaneous determination of simmondsins and simmondsin ferulates in jojoba meal, in detoxified jojoba meal, in jojoba meal extracts, and in animal food mixtures.

Use of laminar chromatographic methods for determination of separation conditions in column extraction chromatography

International Nuclear Information System (INIS)

Ghersini, G.; Cerrai, E.

1978-01-01

Possibilities of using laminar chromatographic methods (paper and thin-layer chromatography) to determine optimal separation conditions in column extraction chromatography are analysed. Most of the given laminar methods are presented as Rf-spectra, i.e. as dependences of Rf found experimentally on eluating solution component concentration. Interrelation between Rf and distribution coefficients of corresponding liquid extraction systems and retention volumes of chromatographic columns is considered. Literature data on extraction paper and thin-layer chromatography of elements with various immovable phases are presented

Enhanced binding by dextran-grafting to Protein A affinity chromatographic media.

Science.gov (United States)

Zhao, Lan; Zhu, Kai; Huang, Yongdong; Li, Qiang; Li, Xiunan; Zhang, Rongyue; Su, Zhiguo; Wang, Qibao; Ma, Guanghui

2017-04-01

Dextran-grafted Protein A affinity chromatographic medium was prepared by grafting dextran to agarose-based matrix, followed by epoxy-activation and Protein A coupling site-directed to sulfhydryl groups of cysteine molecules. An enhancement of both the binding performance and the stability was achieved for this dextran-grafted Protein A chromatographic medium. Its dynamic binding capacity was 61 mg immunoglobulin G/mL suction-dried gel, increased by 24% compared with that of the non-grafted medium. The binding capacity of dextran-grafted medium decreased about 7% after 40 cleaning-in-place cycles, much lower than that of the non-grafted medium as decreased about 15%. Confocal laser scanning microscopy results showed that immunoglobulin G was bound to both the outside and the inside of dextran-grafted medium faster than that of non-grafted one. Atomic force microscopy showed that this dextran-grafted Protein A medium had much rougher surface with a vertical coordinate range of ±80 nm, while that of non-grafted one was ±10 nm. Grafted dextran provided a more stereo surface morphology and immunoglobulin G molecules were more easily to be bound. This high-performance dextran-grafted Protein A affinity chromatographic medium has promising applications in large-scale antibody purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Similarity analyses of chromatographic herbal fingerprints: A review

International Nuclear Information System (INIS)

Goodarzi, Mohammad; Russell, Paul J.; Vander Heyden, Yvan

2013-01-01

Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

Similarity analyses of chromatographic herbal fingerprints: A review

Energy Technology Data Exchange (ETDEWEB)

Goodarzi, Mohammad [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium); Russell, Paul J. [Safety and Environmental Assurance Centre, Unilever, Colworth Science Park, Sharnbrook, Bedfordshire MK44 1LQ (United Kingdom); Vander Heyden, Yvan, E-mail: yvanvdh@vub.ac.be [Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel, Laarbeeklaan 103, B-1090 Brussels (Belgium)

2013-12-04

Graphical abstract: -- Highlights: •Similarity analyses of herbal fingerprints are reviewed. •Different (dis)similarity approaches are discussed. •(Dis)similarity-metrics and exploratory-analysis approaches are illustrated. •Correlation and distance-based measures are overviewed. •Similarity analyses illustrated by several case studies. -- Abstract: Herbal medicines are becoming again more popular in the developed countries because being “natural” and people thus often assume that they are inherently safe. Herbs have also been used worldwide for many centuries in the traditional medicines. The concern of their safety and efficacy has grown since increasing western interest. Herbal materials and their extracts are very complex, often including hundreds of compounds. A thorough understanding of their chemical composition is essential for conducting a safety risk assessment. However, herbal material can show considerable variability. The chemical constituents and their amounts in a herb can be different, due to growing conditions, such as climate and soil, the drying process, the harvest season, etc. Among the analytical methods, chromatographic fingerprinting has been recommended as a potential and reliable methodology for the identification and quality control of herbal medicines. Identification is needed to avoid fraud and adulteration. Currently, analyzing chromatographic herbal fingerprint data sets has become one of the most applied tools in quality assessment of herbal materials. Mostly, the entire chromatographic profiles are used to identify or to evaluate the quality of the herbs investigated. Occasionally only a limited number of compounds are considered. One approach to the safety risk assessment is to determine whether the herbal material is substantially equivalent to that which is either readily consumed in the diet, has a history of application or has earlier been commercialized i.e. to what is considered as reference material. In order

Evaluation of selectivity in homologous multimodal chromatographic systems using in silico designed antibody fragment libraries.

Science.gov (United States)

Karkov, Hanne Sophie; Woo, James; Krogh, Berit Olsen; Ahmadian, Haleh; Cramer, Steven M

2015-12-24

This study describes the in silico design, surface property analyses, production and chromatographic evaluations of a diverse set of antibody Fab fragment variants. Based on previous findings, we hypothesized that the complementarity-determining regions (CDRs) constitute important binding sites for multimodal chromatographic ligands. Given that antibodies are highly diversified molecules and in particular the CDRs, we set out to examine the generality of this result. For this purpose, four different Fab fragments with different CDRs and/or framework regions of the variable domains were identified and related variants were designed in silico. The four Fab variant libraries were subsequently generated by site-directed mutagenesis and produced by recombinant expression and affinity purification to enable examination of their chromatographic retention behavior. The effects of geometric re-arrangement of the functional moieties on the multimodal resin ligands were also investigated with respect to Fab variant retention profiles by comparing two commercially available multimodal cation-exchange ligands, Capto MMC and Nuvia cPrime, and two novel multimodal ligand prototypes. Interestingly, the chromatographic data demonstrated distinct selectivity trends between the four Fab variant libraries. For three of the Fab libraries, the CDR regions appeared as major binding sites for all multimodal ligands. In contrast, the fourth Fab library displayed a distinctly different chromatographic behavior, where Nuvia cPrime and related multimodal ligand prototypes provided markedly improved selectivity over Capto MMC. Clearly, the results illustrate that the discriminating power of multimodal ligands differs between different Fab fragments. The results are promising indications that multimodal chromatography using the appropriate multimodal ligands can be employed in downstream bioprocessing for challenging selective separation of product related variants. Copyright © 2015 Elsevier B

Electrospray[+] tandem quadrupole mass spectrometry in the elucidation of ergot alkaloids chromatographed by HPLC: screening of grass or forage samples for novel toxic compounds.

Science.gov (United States)

Lehner, Andreas F; Craig, Morrie; Fannin, Neil; Bush, Lowell; Tobin, Tom

2005-11-01

Ergot alkaloids are mycotoxins generated by grass and grain pathogens such as Claviceps, for example. Ergot alkaloid-poisoning syndromes, such as tall fescue toxicosis from endophyte-infected tall fescue grass, are important veterinary problems for cattle, horses, sheep, pigs and chickens, with consequent impact on food, meat and dairy industries. Damage to livestock is of the order of a billion dollars a year in the United States alone. HPLC with UV and fluorescence detection are the predominant means of ergot alkaloid determination, with focus on quantitation of the marker compound ergovaline, although ELISA methods are undergoing investigation. These techniques are excellent for rapid detection, but of poor specificity in defining new or poorly characterized ergot alkaloids and related compounds. This paper demonstrates the facility of using electrospray(+) mass spectrometry with multiple reaction monitoring (MRM) detection during chromatographic examination of ergot alkaloid standards of lysergic acid, lysergol, ergonovine, ergovaline, ergotamine, ergocornine, ergocryptine and ergocrystine by HPLC. Ergoline-8 position epimers could be separated on the gradient HPLC system for ergocornine, ergocrystine and ergonovine and appeared as shoulders for ergotamine and ergovaline; epimers generally showed different patterns of relative intensity for specific MRM transitions. There was reasonable correspondence between retention of standards on the 2-mm ESI(+)MS phenyl-hexyl-based reverse phase column and those on the 4-mm C18-based column. Since up to 10% of clinical cases involving toxin exposure display unidentified chromatographic peaks, 11 samples of feed components associated with such cases were studied with developed MRM methods to attempt elucidation of crucial components if possible. Ergotamine appeared in all, ergovaline appeared in five and ergocornine appeared in six; ergonovine, ergocryptine, ergocrystine and lysergol also appeared in several. In addition

Placement of empty catheters for an HDR-emulating LDR prostate brachytherapy technique: comparison to standard intraoperative planning.

Science.gov (United States)

Niedermayr, Thomas R; Nguyen, Paul L; Murciano-Goroff, Yonina R; Kovtun, Konstantin A; Neubauer Sugar, Emily; Cail, Daniel W; O'Farrell, Desmond A; Hansen, Jorgen L; Cormack, Robert A; Buzurovic, Ivan; Wolfsberger, Luciant T; O'Leary, Michael P; Steele, Graeme S; Devlin, Philip M; Orio, Peter F

2014-01-01

We sought to determine whether placing empty catheters within the prostate and then inverse planning iodine-125 seed locations within those catheters (High Dose Rate-Emulating Low Dose Rate Prostate Brachytherapy [HELP] technique) would improve concordance between planned and achieved dosimetry compared with a standard intraoperative technique. We examined 30 consecutive low dose rate prostate cases performed by standard intraoperative technique of planning followed by needle placement/seed deposition and compared them to 30 consecutive low dose rate prostate cases performed by the HELP technique. The primary endpoint was concordance between planned percentage of the clinical target volume that receives at least 100% of the prescribed dose/dose that covers 90% of the volume of the clinical target volume (V100/D90) and the actual V100/D90 achieved at Postoperative Day 1. The HELP technique had superior concordance between the planned target dosimetry and what was actually achieved at Day 1 and Day 30. Specifically, target D90 at Day 1 was on average 33.7 Gy less than planned for the standard intraoperative technique but was only 10.5 Gy less than planned for the HELP technique (p 0.05). Placing empty needles first and optimizing the plan to the known positions of the needles resulted in improved concordance between the planned and the achieved dosimetry to the target, possibly because of elimination of errors in needle placement. Copyright © 2014 American Brachytherapy Society. Published by Elsevier Inc. All rights reserved.

Simple gas chromatographic method for furfural analysis.

Science.gov (United States)

Gaspar, Elvira M S M; Lopes, João F

2009-04-03

A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDfurfurals will contribute to characterise and quantify their presence in the human diet.

Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

Science.gov (United States)

Milina, R.; Mustafa, Z.; Bojilov, D.; Dagnon, S.; Moskovkina, M.

2016-03-01

Pattern recognition method (PRM) was applied to gas chromatographic (GC) data for a fatty acid methyl esters (FAME) composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

Directory of Open Access Journals (Sweden)

Milina R.

2016-03-01

Full Text Available Pattern recognition method (PRM was applied to gas chromatographic (GC data for a fatty acid methyl esters (FAME composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

A Gas Chromatographic System for the Detection of Ethylene Gas Using Ambient Air as a Carrier Gas.

Science.gov (United States)

Zaidi, Nayyer Abbas; Tahir, Muhammad Waseem; Vellekoop, Michael J; Lang, Walter

2017-10-07

Ethylene gas is a naturally occurring gas that has an influence on the shelf life of fruit during their transportation in cargo ships. An unintentional exposure of ethylene gas during transportation results in a loss of fruit. A gas chromatographic system is presented here for the detection of ethylene gas. The gas chromatographic system was assembled using a preconcentrator, a printed 3D printed gas chromatographic column, a humidity sensor, solenoid valves, and an electrochemical ethylene gas sensor. Ambient air was used as a carrier gas in the gas chromatographic system. The flow rate was fixed to 10 sccm. It was generated through a mini-pump connected in series with a mass flow controller. The metal oxide gas sensor is discussed with its limitation in ambient air. The results show the chromatogram obtained from metal oxide gas sensor has low stability, drifts, and has uncertain peaks, while the chromatogram from the electrochemical sensor is stable and precise. Furthermore, ethylene gas measurements at higher ppb concentration and at lower ppb concentration were demonstrated with the electrochemical ethylene gas sensor. The system separates ethylene gas and humidity. The chromatograms obtained from the system are stable, and the results are 1.2% repeatable in five similar measurements. The statistical calculation of the gas chromatographic system shows that a concentration of 2.3 ppb of ethylene gas can be detected through this system.

Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

Science.gov (United States)

Mullett, Wayne M

2007-03-10

The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

Validated electrochemical and chromatographic quantifications of some antibiotic residues in pharmaceutical industrial waste water.

Science.gov (United States)

Ibrahim, Heba K; Abdel-Moety, Mona M; Abdel-Gawad, Sherif A; Al-Ghobashy, Medhat A; Kawy, Mohamed Abdel

2017-03-01

Realistic implementation of ion selective electrodes (ISEs) into environmental monitoring programs has always been a challenging task. This could be largely attributed to difficulties in validation of ISE assay results. In this study, the electrochemical response of amoxicillin trihydrate (AMX), ciprofloxacin hydrochloride (CPLX), trimethoprim (TMP), and norfloxacin (NFLX) was studied by the fabrication of sensitive membrane electrodes belonging to two types of ISEs, which are polyvinyl chloride (PVC) membrane electrodes and glassy carbon (GC) electrodes. Linear response for the membrane electrodes was in the concentration range of 10 -5 -10 -2  mol/L. For the PVC membrane electrodes, Nernstian slopes of 55.1, 56.5, 56.5, and 54.0 mV/decade were achieved over a pH 4-8 for AMX, CPLX, and NFLX, respectively, and pH 3-6 for TMP. On the other hand, for GC electrodes, Nernstian slopes of 59.1, 58.2, 57.0, and 58.2 mV/decade were achieved over pH 4-8 for AMX, CPLX, and NFLX, respectively, and pH 3-6 for TMP. In addition to assay validation to international industry standards, the fabricated electrodes were also cross-validated relative to conventional separation techniques; high performance liquid chromatography (HPLC), and thin layer chromatography (TLC)-densitometry. The HPLC assay was applied in concentration range of 0.5-10.0 μg/mL, for all target analytes. The TLC-densitometry was adopted over a concentration range of 0.3-1.0 μg/band, for AMX, and 0.1-0.9 μg/band, for CPLX, NFLX, and TMP. The proposed techniques were successfully applied for quantification of the selected drugs either in pure form or waste water samples obtained from pharmaceutical plants. The actual waste water samples were subjected to solid phase extraction (SPE) for pretreatment prior to the application of chromatographic techniques (HPLC and TLC-densitometry). On the other hand, the fabricated electrodes were successfully applied for quantification of the antibiotic residues in actual

Coffee contains cholinomimetic compound distinct from caffeine. I: Purification and chromatographic analysis.

Science.gov (United States)

Tse, S Y

1991-07-01

Both regular and decaffeinated coffees were found to have cholinomimetic actions when tested in urethane-anesthetized rats. These actions were distinct from those of caffeine and reversible by atropine. The bioactive fraction was purified from alcoholic extracts of instant decaffeinated coffee by liquid column chromatography and preparative TLC. The purified compound showed similar pharmacological actions as the starting material. Chromatographic behavior was further characterized by analytical TLC and HPLC. Chromatographic analyses of extracts of green coffee beans and roasted ground coffees showed that the cardioactive compound was only present in roasted coffees. Similar analyses of other commonly consumed beverages, including teas and cocoa, showed that this compound was not present in beverages besides coffee.

Quantitation of biological retinoids by high-pressure liquid chromatography: primary internal standardization using tritiated retinoids

International Nuclear Information System (INIS)

Cullum, M.E.; Zile, M.H.

1986-01-01

A single method is described for quantitation of 14 retinoids found in biological material. The method consists of reversed-phase HPLC, internal standardization, and carrier extraction procedures with three synthetic retinoids. Primary standardization of HPLC uv detector is achieved using tritiated all-trans-retinoic acid, all-trans-retinol, all-trans-retinyl palmitate, and all-trans-retinyl acetate. Extraction methods are standardized by correlating the uv absorbance of retinoids at 340 nm with radioactivity of tritiated retinoids of known specific activity. Quantitation of 10 pg of tritiated or 5 ng of nonradioactive retinoid per 0.1 g sample in a polarity range from 4-oxo-retinoic acid to retinyl stearate can be achieved in a single, 50-min chromatographic run. A single HPLC pump, a C 18 reversed-phased analytical column, a multistep three-solvent gradient, and inexpensive solvents based on methanol, water, and chloroform comprise this cost-effective chromatographic system. Our primary standardization method allows investigators employing different procedures to compare results between laboratories by standardizing the HPLC uv detector with commercially available tritiated retinoids. With this method we were able to quantitate nanomolar amounts of endogenous retinoic acids and retinyl esters, that HPLC uv only conditions usually would not detect in the circulation and liver of rats under physiological conditions

ChromAlign: A two-step algorithmic procedure for time alignment of three-dimensional LC-MS chromatographic surfaces.

Science.gov (United States)

Sadygov, Rovshan G; Maroto, Fernando Martin; Hühmer, Andreas F R

2006-12-15

We present an algorithmic approach to align three-dimensional chromatographic surfaces of LC-MS data of complex mixture samples. The approach consists of two steps. In the first step, we prealign chromatographic profiles: two-dimensional projections of chromatographic surfaces. This is accomplished by correlation analysis using fast Fourier transforms. In this step, a temporal offset that maximizes the overlap and dot product between two chromatographic profiles is determined. In the second step, the algorithm generates correlation matrix elements between full mass scans of the reference and sample chromatographic surfaces. The temporal offset from the first step indicates a range of the mass scans that are possibly correlated, then the correlation matrix is calculated only for these mass scans. The correlation matrix carries information on highly correlated scans, but it does not itself determine the scan or time alignment. Alignment is determined as a path in the correlation matrix that maximizes the sum of the correlation matrix elements. The computational complexity of the optimal path generation problem is reduced by the use of dynamic programming. The program produces time-aligned surfaces. The use of the temporal offset from the first step in the second step reduces the computation time for generating the correlation matrix and speeds up the process. The algorithm has been implemented in a program, ChromAlign, developed in C++ language for the .NET2 environment in WINDOWS XP. In this work, we demonstrate the applications of ChromAlign to alignment of LC-MS surfaces of several datasets: a mixture of known proteins, samples from digests of surface proteins of T-cells, and samples prepared from digests of cerebrospinal fluid. ChromAlign accurately aligns the LC-MS surfaces we studied. In these examples, we discuss various aspects of the alignment by ChromAlign, such as constant time axis shifts and warping of chromatographic surfaces.

Liquid chromatographic method for determining the concentration of bisazir in water

Science.gov (United States)

Scholefield, Ronald J.; Slaght, Karen S.; Allen, John L.

1997-01-01

Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys (Petromyzon marinus) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)-N-methylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a C18 column, a mobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).

Inductively coupled plasma emission spectrometric detection of simulated high performance liquid chromatographic peaks

International Nuclear Information System (INIS)

Fraley, D.M.; Yates, D.; Manahan, S.E.

1979-01-01

Because of its multielement capability, element-specificity, and low detection limits, inductively coupled plasma optical emission spectrometry (ICP) is a very promising technique for the detection of specific elemental species separated by high performance liquid chromatography (HPLC). This paper evaluated ICP as a detector for HPLC peaks containing specific elements. Detection limits for a number of elements have been evaluated in terms of the minimum detectable concentration of the element at the chromatographic peak maximum. The elements studies were Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sr, Ti, V, and Zn. In addition, ICP was compared with atomic absorption spectrometry for the detection of HPLC peaks composed of EDTA and NTA chelates of copper. Furthermore, ICP was compared to uv solution absorption for the detection of copper chelates. 6 figures, 4 tables

Preparation, chromatographic evaluation and biodistribution of "9"9"mTc-procainamide as a radiopharmaceutical for heart imaging

International Nuclear Information System (INIS)

Motaleb, M.A.; Ibrahim, I.T.; Abo Rizq, R.S.; Elzanfaly, E.S.

2017-01-01

Procainamide (4-amino-N-[2-(diethylamino) ethyl] benzamide) is a sodium channel blocker, which acts as an effective antiarrhythmic agent used in the treatment of a variety of atrial and ventricular arrhythmias. The aim of this study was to prepare "9"9"mTc-procainamide complex, apply different chromatographic techniques for the assay of radiolabeling yield and study its biodistribution as a novel radiopharmaceutical for heart imaging. "9"9"mTc-procainamide was obtained with a maximum labeling yield of 95.76±0.20% via direct labeling method under optimum conditions of 200 μg of procainamide, 300 μL of buffer (carbonate) at pH 11, 30 μg SnCl_2 . 2H_2O at room temperature (25 C) for 15 min. In terms of in vitro stability, the complex was stable for 3 h. Chromatographic evaluation using paper chromatography, thin layer chromatography, gel chromatography, and high performance liquid chromatography showed reliable results for measuring the radiochemical yield. Biodistribution study of "9"9"mTc-procainamide showed ratios of heart/lung and heart/liver (6.38±1.50, 2.06±0.31, respectively at 30 min post injection) which was comparable to that of "9"9"mTc-sestamibi (7.4±2.00, 0.97±0.10, respectively at 60 min, P<0.05).

Preparation, chromatographic evaluation and biodistribution of {sup 99m}Tc-procainamide as a radiopharmaceutical for heart imaging

Energy Technology Data Exchange (ETDEWEB)

Motaleb, M.A.; Ibrahim, I.T.; Abo Rizq, R.S. [Atomic Energy Authority, Cairo (Egypt). Labeled Compound Dept.; Elzanfaly, E.S. [Cairo Univ. (Egypt). Analytical Dept.

2017-06-01

Procainamide (4-amino-N-[2-(diethylamino) ethyl] benzamide) is a sodium channel blocker, which acts as an effective antiarrhythmic agent used in the treatment of a variety of atrial and ventricular arrhythmias. The aim of this study was to prepare {sup 99m}Tc-procainamide complex, apply different chromatographic techniques for the assay of radiolabeling yield and study its biodistribution as a novel radiopharmaceutical for heart imaging. {sup 99m}Tc-procainamide was obtained with a maximum labeling yield of 95.76±0.20% via direct labeling method under optimum conditions of 200 μg of procainamide, 300 μL of buffer (carbonate) at pH 11, 30 μg SnCl{sub 2} . 2H{sub 2}O at room temperature (25 C) for 15 min. In terms of in vitro stability, the complex was stable for 3 h. Chromatographic evaluation using paper chromatography, thin layer chromatography, gel chromatography, and high performance liquid chromatography showed reliable results for measuring the radiochemical yield. Biodistribution study of {sup 99m}Tc-procainamide showed ratios of heart/lung and heart/liver (6.38±1.50, 2.06±0.31, respectively at 30 min post injection) which was comparable to that of {sup 99m}Tc-sestamibi (7.4±2.00, 0.97±0.10, respectively at 60 min, P<0.05).

Detection and quantification of ginsenoside Re in ginseng samples by a chromatographic immunostaining method using monoclonal antibody against ginsenoside Re.

Science.gov (United States)

Morinaga, Osamu; Tanaka, Hiroyuki; Shoyama, Yukihiro

2006-01-02

A chromatographic immunostaining method has been developed for the determination of ginsenoside Re (G-Re) in ginseng samples on a polyethersulphone (PES) membrane. G-Re standard and the extracts of ginseng roots were applied to a PES membrane and developed by methanol-water-acetic acid (45:55:1, by volume). G-Re was clearly detected by an immunostaining method using a monoclonal antibody against G-Re. The coloring spots of G-Re were analyzed quantitatively using NIH Image software indicating at least 0.125 microg of G-Re was detectable. G-Re can be analyzed quantitatively between 0.25 and 4.0 microg.

Radio-chromatographic determination of plasmatic adenosine deaminase (A.D.)

International Nuclear Information System (INIS)

Chivot, J.J.; Depernet, D.; Caen, J.

1970-01-01

We were able, by using a radio-chromatographic method, to measure an adenosine deaminase activity in normal human heparinized platelet-poor plasma, which can degrade 0.016 μM adenosine. This activity suppressed by heating 56 C for 30 minutes is inhibited by high concentrations of urea and is proportional to the amount of plasma, source of enzyme, in the systems. (authors) [fr

Ground-based intercomparison of two isoprene measurement techniques

Directory of Open Access Journals (Sweden)

E. Leibrock

2003-01-01

Full Text Available An informal intercomparison of two isoprene (C5H8 measurement techniques was carried out during Fall of 1998 at a field site located approximately 3 km west of Boulder, Colorado, USA. A new chemical ionization mass spectrometric technique (CIMS was compared to a well-established gas chromatographic technique (GC. The CIMS technique utilized benzene cation chemistry to ionize isoprene. The isoprene levels measured by the CIMS were often larger than those obtained with the GC. The results indicate that the CIMS technique suffered from an anthropogenic interference associated with air masses from the Denver, CO metropolitan area as well as an additional interference occurring in clean conditions. However, the CIMS technique is also demonstrated to be sensitive and fast. Especially after introduction of a tandem mass spectrometric technique, it is therefore a candidate for isoprene measurements in remote environments near isoprene sources.

Radiographic analysis of the temporomandibular joint by the standardized projection technique

International Nuclear Information System (INIS)

Choe, Han Up; Park, Tae Won

1983-01-01

The purpose of this study was to investigate the radiographic images of the condylar head in clinically normal subjects and the TMJ patients using standardized projection technique. 45 subjects who have not clinical evidence of TMJ problems and 96 patients who have the clinical evidence of TMJ problems were evaluated, but the patients who had fracture, trauma and tumor on TMJ area were discluded in this study. For the evaluation of radiographic images, the author has observed the condylar head positions in closed mouth and 2.54 cm open mouth position taken by the standardized transcranial oblique lateral projection technique. The results were as follow: 1. In closed mouth position, the crest of condylar head took relatively posterior position to the deepest point of the glenoid fossa in 8.9% of the normals and in 26.6% of TMJ patients. 2. In 2.54 cm open mouth position, condylar head took relatively posterior position to the articular eminence in 2 .2% of TMJ patients and 39.6% of the normals. 3. In open mouth position, the horizontal distance from the deepest point of the glenoid fossa to the condylar head was 13.96 mm in the normals and 10.68 mm in TMJ patients. 4. The distance of true movement of condylar head was 13.49 mm in the normals and 10.27 mm in TMJ patients. 5. The deviation of mandible in TMJ patients was slightly greater than of the normals.

A standardized method for the calibration of thermodynamic data for the prediction of gas chromatographic retention times.

Science.gov (United States)

McGinitie, Teague M; Ebrahimi-Najafabadi, Heshmatollah; Harynuk, James J

2014-02-21

A new method for calibrating thermodynamic data to be used in the prediction of analyte retention times is presented. The method allows thermodynamic data collected on one column to be used in making predictions across columns of the same stationary phase but with varying geometries. This calibration is essential as slight variances in the column inner diameter and stationary phase film thickness between columns or as a column ages will adversely affect the accuracy of predictions. The calibration technique uses a Grob standard mixture along with a Nelder-Mead simplex algorithm and a previously developed model of GC retention times based on a three-parameter thermodynamic model to estimate both inner diameter and stationary phase film thickness. The calibration method is highly successful with the predicted retention times for a set of alkanes, ketones and alcohols having an average error of 1.6s across three columns. Copyright © 2014 Elsevier B.V. All rights reserved.

Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

International Nuclear Information System (INIS)

Luca, Michele De; Ragno, Gaetano; Ioele, Giuseppina; Tauler, Romà

2014-01-01

Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described

Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

Energy Technology Data Exchange (ETDEWEB)

Luca, Michele De, E-mail: michele.deluca@unical.it [Department of Pharmacy, Health and Nutritional Sciences, University of Calabria, Via P. Bucci, Rende, CS 87036 (Italy); Ragno, Gaetano; Ioele, Giuseppina [Department of Pharmacy, Health and Nutritional Sciences, University of Calabria, Via P. Bucci, Rende, CS 87036 (Italy); Tauler, Romà [Department of Environmental Chemistry, IDAEA-CSIC, C/Jordi Girona, 18-26, Barcelona 08034 (Spain)

2014-07-21

Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described.

Techniques for rapid determination of effects of synergy between radionuclides and pollutants

International Nuclear Information System (INIS)

Saas, A.; Grauby, A.

1975-01-01

The authors present a number of chromatographic techniques for rapid determination of synergy between radionuclides and various compounds in water. The first technique consists in studying how the chemical equilibrium of iodine varies in the presence of various organic and mineral compounds. The second makes it possible to define the effects of synergy within a given hydrographic basin. A third technique deals with the effects of synergy in ground water in the presence of various types of irrigation water. Finally, to complete this set of techniques, the authors define the mobility potential of a radionuclide in a given aqueous effluent

Chemometrics and chromatographic fingerprints to classify plant food supplements according to the content of regulated plants.

Science.gov (United States)

Deconinck, E; Sokeng Djiogo, C A; Courselle, P

2017-09-05

Plant food supplements are gaining popularity, resulting in a broader spectrum of available products and an increased consumption. Next to the problem of adulteration of these products with synthetic drugs the presence of regulated or toxic plants is an important issue, especially when the products are purchased from irregular sources. This paper focusses on this problem by using specific chromatographic fingerprints for five targeted plants and chemometric classification techniques in order to extract the important information from the fingerprints and determine the presence of the targeted plants in plant food supplements in an objective way. Two approaches were followed: (1) a multiclass model, (2) 2-class model for each of the targeted plants separately. For both approaches good classification models were obtained, especially when using SIMCA and PLS-DA. For each model, misclassification rates for the external test set of maximum one sample could be obtained. The models were applied to five real samples resulting in the identification of the correct plants, confirmed by mass spectrometry. Therefore chromatographic fingerprinting combined with chemometric modelling can be considered interesting to make a more objective decision on whether a regulated plant is present in a plant food supplement or not, especially when no mass spectrometry equipment is available. The results suggest also that the use of a battery of 2-class models to screen for several plants is the approach to be preferred. Copyright © 2017 Elsevier B.V. All rights reserved.

Compressed air injection technique to standardize block injection pressures.

Science.gov (United States)

Tsui, Ban C H; Li, Lisa X Y; Pillay, Jennifer J

2006-11-01

Presently, no standardized technique exists to monitor injection pressures during peripheral nerve blocks. Our objective was to determine if a compressed air injection technique, using an in vitro model based on Boyle's law and typical regional anesthesia equipment, could consistently maintain injection pressures below a 1293 mmHg level associated with clinically significant nerve injury. Injection pressures for 20 and 30 mL syringes with various needle sizes (18G, 20G, 21G, 22G, and 24G) were measured in a closed system. A set volume of air was aspirated into a saline-filled syringe and then compressed and maintained at various percentages while pressure was measured. The needle was inserted into the injection port of a pressure sensor, which had attached extension tubing with an injection plug clamped "off". Using linear regression with all data points, the pressure value and 99% confidence interval (CI) at 50% air compression was estimated. The linearity of Boyle's law was demonstrated with a high correlation, r = 0.99, and a slope of 0.984 (99% CI: 0.967-1.001). The net pressure generated at 50% compression was estimated as 744.8 mmHg, with the 99% CI between 729.6 and 760.0 mmHg. The various syringe/needle combinations had similar results. By creating and maintaining syringe air compression at 50% or less, injection pressures will be substantially below the 1293 mmHg threshold considered to be an associated risk factor for clinically significant nerve injury. This technique may allow simple, real-time and objective monitoring during local anesthetic injections while inherently reducing injection speed.

Detection of irradiated fruits and vegetables by gas-chromatographic methods and electron spin-resonance

Energy Technology Data Exchange (ETDEWEB)

Farag, S.E.A. (National Centre for Radiation Research and Technology, Cairo (Egypt))

1993-01-01

Gas chromatographic methods detected some hydrocarbons esp. 17:1, 16:2, 15:0 and 14:1 in irradiated, Avocado, Papaya, Mangoes with 0.75, 1.5, 3.0 kGy and Apricot with 0.5 and 3.0 kGy. The detection of hydrocarbons was clearly at high doses but the low doses need more sensitive conditions using Liquid-Liquid-Gas chromatographic method as used here. Using Electron Spin-Resonance, produce a specific signal from irradiated onion (dried leaves) as well as apricot (hard coat of kernels) after some weeks of irradiation process but not clear with the other foodstuffs. (orig.)

Investigations for chromatographic separation and determination of the rare earths and auxiliary group elements

International Nuclear Information System (INIS)

Post, K.

1981-01-01

Different method have been developed to quantitatively determine rare earth elements after their column chromatographic separation. The influence of the active solvents in the running systems diethyl ether/tetra hydrofuran (THF)/nitric acid (HNO 3 ) and diethyl ether/bis-(2-ethyl hexyl) phosphate (HDEHP)/HNO 3 was investigated on the column chromatographic separation of all rare earth elements is possible by the synergistic combination of the active running components THF and HDEHP. Further from product isotopes could also be separated using the running agents described here in investigations to separate fission product mixtures of irradiated uranium. (orig./HBR) [de

Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

OpenAIRE

Hassib, Sonia T.; Farag, Awatef E.; Elkady, Ehab F.

2011-01-01

Simple, accurate and precise reversed-phase liquid chromatographic (LC) and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS) and trimethoprim (TMP) in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm) based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9):acetonitrile:water (25:100:50, v/v/v) at a flow rate of 1...

Gas chromatographic column for the Viking 1975 molecular analysis experiment

Science.gov (United States)

Novotny, M.; Hayes, J. M.; Bruner, F.; Simmonds, P. G.

1975-01-01

A gas chromatographic column has been developed for use in the remote analysis of the Martian surface. The column, which utilizes a liquid-modified organic adsorbent (Tenax) as the stationary phase, provides efficient transmission and resolution of nanogram quantities of organic materials in the presence of millionfold excesses of water and carbon dioxide.

Gas chromatographic determination of calcium propionate added as preservative to bread.

Science.gov (United States)

Lamkin, W M; Unruh, N C; Pomeranz, Y

1987-01-01

A simple and rapid gas chromatographic procedure was developed for determining low concentrations of propionate added as a preservative to bread. A bread sample to be analyzed was ground in a meat grinder with a 3 mm hole plate and finely divided by rubbing through a No. 8 sieve. The propionate was then extracted into 0.050M formic acid in a blender at low speed for 5 min, and an aliquot of a filtrate was analyzed directly by gas chromatography. Chromatographic separation was accomplished on a Carbopack C column coated with 0.3% (w/w) Carbowax 20M and 0.1% (w/w) phosphoric acid. Less than 0.2 ppm propionic acid could be detected in the aqueous extract. Over the range of 0.03-0.23% calcium propionate, average relative error was -1.20% with an average coefficient of variation of 2.02%.

Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

Science.gov (United States)

Wang, Xuan; Ye, Nengsheng

2017-12-01

In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validated high-performance thin-layer chromatographic (HPTLC method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate cream using fractional factorial design

Directory of Open Access Journals (Sweden)

Kalpana G. Patel

2016-07-01

Full Text Available A high-performance thin-layer chromatographic method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate was developed and validated as per International Conference on Harmonization guidelines. High-performance thin-layer chromatographic separation was performed on aluminum plates precoated with silica gel 60F254 and methanol:ethyl acetate:toluene: acetonitrile:3M ammonium formate in water (1:2.5:6.0:0.3:0.2, % v/v as optimized mobile phase at detection wavelength of 224 nm. The retardation factor (Rf values for nadifloxacin, mometasone furoate, and miconazole nitrate were 0.23, 0.70, and 0.59, respectively. Percent recoveries in terms of accuracy for the marketed formulation were found to be 98.35–99.76%, 99.36–99.65%, and 99.16–100.25% for nadifloxacin, mometasone furoate, and miconazole nitrate, respectively. The pooled percent relative standard deviation for repeatability and intermediate precision studies was found to be < 2% for three target analytes. The effect of four independent variables, methanol content in total mobile phase, wavelength, chamber saturation time, and solvent front, was evaluated by fractional factorial design for robustness testing. Amongst all four factors, volume of methanol in mobile phase appeared to have a possibly significant effect on retention factor of miconazole nitrate compared with the other two drugs nadifloxacin and mometasone furoate, and therefore it was important to be carefully controlled. In summary, a novel, simple, accurate, reproducible, and robust high-performance thin-layer chromatographic method was developed, which would be of use in quality control of these cream formulations.

Gas chromatographic determination of impurities of inorganic compounds

International Nuclear Information System (INIS)

Drugov, Yu.S.

1985-01-01

Methods of concentration, separation, detection in gas chromatographic determination of impurities of inorganic compounds including low-boiling gases, reactive gases, organometallic compounds, free metals, anions, etc. are reviewed. Methods of reaction gas chromatography for determining reactive gases, water, anions, metal chelates are considered in detail as well as methods of reaction-sorption concentration and reaction gas extraction. The application of gas chromatograpny ior anaiysis of water and atmosphere contamination, for determination of impurities in highly pure solid substances and gases is described

MATLAB Toolboxes for Reference Electrode Standardization Technique (REST) of Scalp EEG.

Science.gov (United States)

Dong, Li; Li, Fali; Liu, Qiang; Wen, Xin; Lai, Yongxiu; Xu, Peng; Yao, Dezhong

2017-01-01

Reference electrode standardization technique (REST) has been increasingly acknowledged and applied as a re-reference technique to transform an actual multi-channels recordings to approximately zero reference ones in electroencephalography/event-related potentials (EEG/ERPs) community around the world in recent years. However, a more easy-to-use toolbox for re-referencing scalp EEG data to zero reference is still lacking. Here, we have therefore developed two open-source MATLAB toolboxes for REST of scalp EEG. One version of REST is closely integrated into EEGLAB, which is a popular MATLAB toolbox for processing the EEG data; and another is a batch version to make it more convenient and efficient for experienced users. Both of them are designed to provide an easy-to-use for novice researchers and flexibility for experienced researchers. All versions of the REST toolboxes can be freely downloaded at http://www.neuro.uestc.edu.cn/rest/Down.html, and the detailed information including publications, comments and documents on REST can also be found from this website. An example of usage is given with comparative results of REST and average reference. We hope these user-friendly REST toolboxes could make the relatively novel technique of REST easier to study, especially for applications in various EEG studies.

Comparison of twin-cell centrifugal partition chromatographic columns with different cell volume.

Science.gov (United States)

Goll, Johannes; Audo, Gregoire; Minceva, Mirjana

2015-08-07

Two twin-cell centrifugal partition chromatographic columns (SCPC 250 and SCPE-250-BIO, Armen Instrument, France) with the same column volume but different cell size and number were compared in terms of stationary phase retention and column efficiency. The columns were tested with two types of solvent systems: a commonly used organic solvent based biphasic system from the ARIZONA solvent system family and a polymer/salt based aqueous two phase system (ATPS). The efficiency of the columns was evaluated by pulse injection experiments of two benzenediols (pyrocatechol and hydroquinone) in the case of the ARIZONA system and a protein mixture (myoglobin and lysozyme) in the case of the ATPS. As result of high stationary phase retention, the column with the lower number of larger twin-cells (SCPE-250-BIO) is suitable for protein separations using ATPS. On the other hand, due to higher column efficiency, the column with the greater number of smaller cells (SCPC 250) is superior for batch elution separations performed with standard liquid-liquid chromatography organic solvent based biphasic systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Gas chromatographic-mass spectrometric determination of hydrophilic compounds in environmental water by solid-phase extraction with activated carbon fiber felt.

Science.gov (United States)

Kawata, K; Ibaraki, T; Tanabe, A; Yagoh, H; Shinoda, A; Suzuki, H; Yasuhara, A

2001-03-09

Simple gas chromatographic-mass spectrometric determination of hydrophilic organic compounds in environmental water was developed. A cartridge containing activated carbon fiber felt was made by way of trial and was evaluated for solid-phase extraction of the compounds in water. The hydrophilic compounds investigated were acrylamide, N,N-dimethylacetamide, N,N-dimethylformamide, 1,4-dioxane, furfural, furfuryl alcohol, N-nitrosodiethylamine and N-nitrosodimethylamine. Overall recoveries were good (80-100%) from groundwater and river water. The relative standard deviations ranged from 4.5 to 16% for the target compounds. The minimum detectable concentrations were 0.02 to 0.03 microg/l. This method was successfully applied to several river water samples.

New liquid chromatographic-chemometric approach for the determination of sunset yellow and tartrazine in commercial preparation.

Science.gov (United States)

Dinç, Erdal; Aktaş, A Hakan; Ustündağ, Ozgür

2005-01-01

A new liquid chromatographic (LC)-chemometric approach was developed for the determination of sunset yellow (SUN) and tartrazine (TAR) in commercial preparations. This approach uses LC and chemometric calibration methods, i.e., classical least-squares (CLS), principal component regression (PCR), and partial-least squares (PLS), simultaneously. The combined LC-chemometric approaches, denoted as LC-CLS, LC-PCR, and LC-PLS, are based on photodiode array (PDA) detection at multiple wavelengths. Optimum chromatographic separation of SUN and TAR with allura red as the internal standard (IS) was obtained by using a Waters Symmetry C18 column, 5 microm, 4.6 x 250 mm, and 0.2 M acetate buffer (pH 5)-acetonitrile-methano-bidistilled water (55 + 20 + 15 + 10, v/v) as the mobile phase at a flow rate of 1.9 mL/min. The LC data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using PDA detection at 5 wavelengths (465, 470, 475, 480, and 485 nm). LC-chemometric calibrations for SUN and TAR were separately constructed by using the relationship between the peak-area ratio and the training sets for each colorant. LC-chemometric approaches were tested for different synthetic mixtures containing SUN and TAR in the presence of the IS. These LC-chemometric calibrations were applied to a commercial preparation of the 2 colorants. The experimental results of the LC-chemometric approaches were compared with those obtained by a developed classical LC method using single-wavelength detection.

Porous chromatographic materials as substrates for preparing synthetic nuclear explosion debris particles

International Nuclear Information System (INIS)

Harvey, S.D.; Carman, A.J.; Martin Liezers; Antolick, K.C.; Garcia, B.J.; Eiden, G.C.; Sweet, L.E.

2013-01-01

Several porous chromatographic materials were investigated as synthetic substrates for preparing surrogate nuclear explosion debris particles. Eighteen metals, including some of forensic interest, were loaded onto materials by immersing them in metal solutions (556 mg/L of each metal) to fill the pores, applying gentle heat (110 deg C) to drive off water, and then treating them at high temperatures (up to 800 deg C) in air to form less soluble metal species. High-boiling-point metals were uniformly loaded on spherical controlled-pore glass to emulate early fallout, whereas low-boiling-point metals were loaded on core-shell silica to represent coated particles formed later in the nuclear fallout-formation process. Analytical studies characterized material balance and the formation of recalcitrant species. Metal loading was 1.5-3 times higher than expected from the pore volume alone, a result attributed to surface coating. Most metals were passively loaded; that is, solutions filled the pores without active metal discrimination. However, niobium and tin concentrations were lower in solutions after pore filling, and were found in elevated concentrations in the final products, indicating selective loading. High-temperature treatments caused reduced solubility of several metals, and the loss of some volatile species (rhenium and tellurium). Sample preparation reproducibility was high (the inter- and intra-batch relative standard deviations were 7.8 and 0.84 %, respectively) indicating suitability for use as a working standard for analytical methods development. We anticipate future standardized radionuclide-loaded materials will find use in radioanalytical methods development and/or serve as a starting material for the synthesis of more complex nuclear explosion debris forms (e.g., Trinitite). (author)

Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

Science.gov (United States)

Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

2006-01-01

A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

Identification of vegetable oil botanical speciation in refined vegetable oil blends using an innovative combination of chromatographic and spectroscopic techniques.

Science.gov (United States)

Osorio, Maria Teresa; Haughey, Simon A; Elliott, Christopher T; Koidis, Anastasios

2015-12-15

European Regulation 1169/2011 requires producers of foods that contain refined vegetable oils to label the oil types. A novel rapid and staged methodology has been developed for the first time to identify common oil species in oil blends. The qualitative method consists of a combination of a Fourier Transform Infrared (FTIR) spectroscopy to profile the oils and fatty acid chromatographic analysis to confirm the composition of the oils when required. Calibration models and specific classification criteria were developed and all data were fused into a simple decision-making system. The single lab validation of the method demonstrated the very good performance (96% correct classification, 100% specificity, 4% false positive rate). Only a small fraction of the samples needed to be confirmed with the majority of oils identified rapidly using only the spectroscopic procedure. The results demonstrate the huge potential of the methodology for a wide range of oil authenticity work. Copyright © 2014 Elsevier Ltd. All rights reserved.

A high performance liquid chromatographic assay of Mefloquine in saliva after a single oral dose in healthy adult Africans

Directory of Open Access Journals (Sweden)

Gbotosho Grace O

2012-02-01

Full Text Available Abstract Background Mefloquine-artesunate is a formulation of artemisinin based combination therapy (ACT recommended by the World Health Organization and historically the first ACT used clinically. The use of ACT demands constant monitoring of therapeutic efficacies and drug levels, in order to ensure that optimum drug exposure is achieved and detect reduced susceptibility to these drugs. Quantification of anti-malarial drugs in biological fluids other than blood would provide a more readily applicable method of therapeutic drug monitoring in developing endemic countries. Efforts in this study were devoted to the development of a simple, field applicable, non-invasive method for assay of mefloquine in saliva. Methods A high performance liquid chromatographic method with UV detection at 220 nm for assaying mefloquine in saliva was developed and validated by comparing mefloquine concentrations in saliva and plasma samples from four healthy volunteers who received single oral dose of mefloquine. Verapamil was used as internal standard. Chromatographic separation was achieved using a Hypersil ODS column. Results Extraction recoveries of mefloquine in plasma or saliva were 76-86% or 83-93% respectively. Limit of quantification of mefloquine was 20 ng/ml. Agreement between salivary and plasma mefloquine concentrations was satisfactory (r = 0.88, p Conclusion Disposition of mefloquine in saliva paralleled that in plasma, making salivary quantification of mefloquine potentially useful in therapeutic drug monitoring.

Ion chromatographic determination of vanadium (4) and vanadium (5) in the form of EDTA complexes

International Nuclear Information System (INIS)

Komarova, T.V.; Obrezkov, O.N.; Shpigun, O.A.

1991-01-01

Ion chromatographic behaviour of V 4+ and V 5+ -EDTA complexes (1,2) and V 5+ -EDTA monoperoxo complexes (3) has been studied. The regularities of ion exchange are obeyed for 1 and 3 complexes. These complex anions are strongly retained on HIX-1 anion exchanger. The chromatographic characteristics of 2 change in time, therefore its determination is impossible under the conditions studied. A method has been developed of the simultaneous determination of V 4+ and V 5+ which is based on retarded formation of the V 5+ -EDTA monoperoxo complex in a system of V 4+ -EDTA - H 2 O 2

The contribution of the hydrogen bond acidity on the lipophilicity of drugs estimated from chromatographic measurements.

Science.gov (United States)

Pallicer, Juan M; Pascual, Rosalia; Port, Adriana; Rosés, Martí; Ràfols, Clara; Bosch, Elisabeth

2013-02-14

The influence of the hydrogen bond acidity when the 1-octanol/water partition coefficient (log P(o/w)) of drugs is determined from chromatographic measurements was studied in this work. This influence was firstly evaluated by means of the comparison between the Abraham solvation parameter model when it is applied to express the 1-octanol/water partitioning and the chromatographic retention, expressed as the solute polarity p. Then, several hydrogen bond acidity descriptors were compared in order to determine properly the log P(o/w) of drugs. These descriptors were obtained from different software and comprise two-dimensional parameters such as the calculated Abraham hydrogen bond acidity A and three-dimensional descriptors like HDCA-2 from CODESSA program or WO1 and DRDODO descriptors calculated from Volsurf+software. The additional HOMO-LUMO polarizability descriptor should be added when the three-dimensional descriptors are used to complement the chromatographic retention. The models generated using these descriptors were compared studying the correlations between the determined log P(o/w) values and the reference ones. The comparison showed that there was no significant difference between the tested models and any of them was able to determine the log P(o/w) of drugs from a single chromatographic measurement and the correspondent molecular descriptors terms. However, the model that involved the calculated A descriptor was simpler and it is thus recommended for practical uses. Copyright © 2012 Elsevier B.V. All rights reserved.

Standard practice for monitoring atmospheric SO2 using the sulfation plate technique

CERN Document Server

American Society for Testing and Materials. Philadelphia

1997-01-01

1.1 This practice covers a weighted average effective SO2 level for a 30-day interval through the use of the sulfation plate method, a technique for estimating the effective SO2 content of the atmosphere, and especially with regard to the atmospheric corrosion of stationary structures or panels. This practice is aimed at determining SO2 levels rather than sulfuric acid aerosol or acid precipitation. 1.2 The results of this practice correlate approximately with volumetric SO2 concentrations, although the presence of dew or condensed moisture tends to enhance the capture of SO2 into the plate. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

Assessment of chromatographic methods for the chemical stability of a new miconazole nitrate cream

International Nuclear Information System (INIS)

Garcia Pulpeiro, Oscar; Calzadilla Aguiar, Wendy; Rodriguez Bencomo, Wendy

2013-01-01

To assess the chromatographic methods for the chemical stability of a new 2 % miconazol nitrate cream. arious degradation conditions were firstly used in the raw material miconazole nitrate in order to obtain the possible degradation products of this drug and to evaluate them by thin layer chromatography-based method, which was validated to identify the degradation products in the new cream. The performance of the official method based on high resolution liquid chromatography and reported in British Pharmacopoeia 2010 was evaluated, and its selectivity against the possible degradation products were also analyzed. Both chromatographic methods were applied to the analysis of cream samples from the three pilot batches under heat stress for 30 days

Leveraging probabilistic peak detection to estimate baseline drift in complex chromatographic samples

NARCIS (Netherlands)

Lopatka, M.; Barcaru, A.; Sjerps, M.J.; Vivó-Truyols, G.

2016-01-01

Accurate analysis of chromatographic data often requires the removal of baseline drift. A frequently employed strategy strives to determine asymmetric weights in order to fit a baseline model by regression. Unfortunately, chromatograms characterized by a very high peak saturation pose a significant

Comparison of chromatographic methods for the determination of bound glycerol in biodiesel

Energy Technology Data Exchange (ETDEWEB)

Foglia, T.A.; Jones, K.C.; Nunez, A.; Phillips, J.G. [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA (United States); Mittelbach, M. [Inst. for Chemistry, Univ. of Graz, Graz (Austria)

2004-09-01

An important fuel criterion for biodiesel is bound glycerol, which is a function of the residual amount of triglycerides and partial glycerides in the biodiesel. Either high-temperature gas chromatography or high performance liquid chromatography can be used for determining these minor but important components in biodiesel. In this paper we have conducted a statistical study on the accuracy of the two methods for ascertaining the bound glycerol in biodiesel fuels obtained from different feedstocks. Analysis of variance showed that with one exception, namely diacylglycerols in some soy oil based biodiesel, there was no statistical difference in bound glycerol for the biodiesel samples analyzed or a difference between methods. Operationally, the high performance liquid chromatographic method is superior to the high temperature gas chromatographic method in that it requires no sample derivatization, has shorter analysis times, and is directly applicable to most biodiesel fuels. (orig.)

Assessing the service quality of Iran military hospitals: Joint Commission International standards and Analytic Hierarchy Process (AHP) technique

Science.gov (United States)

Bahadori, Mohammadkarim; Ravangard, Ramin; Yaghoubi, Maryam; Alimohammadzadeh, Khalil

2014-01-01

Background: Military hospitals are responsible for preserving, restoring and improving the health of not only armed forces, but also other people. According to the military organizations strategy, which is being a leader and pioneer in all areas, providing quality health services is one of the main goals of the military health care organizations. This study was aimed to evaluate the service quality of selected military hospitals in Iran based on the Joint Commission International (JCI) standards and comparing these hospitals with each other and ranking them using the analytic hierarchy process (AHP) technique in 2013. Materials and Methods: This was a cross-sectional and descriptive study conducted on five military hospitals, selected using the purposive sampling method, in 2013. Required data collected using checklists of accreditation standards and nominal group technique. AHP technique was used for prioritizing. Furthermore, Expert Choice 11.0 was used to analyze the collected data. Results: Among JCI standards, the standards of access to care and continuity of care (weight = 0.122), quality improvement and patient safety (weight = 0.121) and leadership and management (weight = 0.117) had the greatest importance, respectively. Furthermore, in the overall ranking, BGT (weight = 0.369), IHM (0.238), SAU (0.202), IHK (weight = 0.125) and SAB (weight = 0.066) ranked first to fifth, respectively. Conclusion: AHP is an appropriate technique for measuring the overall performance of hospitals and their quality of services. It is a holistic approach that takes all hospital processes into consideration. The results of the present study can be used to improve hospitals performance through identifying areas, which are in need of focus for quality improvement and selecting strategies to improve service quality. PMID:25250364

Assessing the service quality of Iran military hospitals: Joint Commission International standards and Analytic Hierarchy Process (AHP) technique.

Science.gov (United States)

Bahadori, Mohammadkarim; Ravangard, Ramin; Yaghoubi, Maryam; Alimohammadzadeh, Khalil

2014-01-01

Military hospitals are responsible for preserving, restoring and improving the health of not only armed forces, but also other people. According to the military organizations strategy, which is being a leader and pioneer in all areas, providing quality health services is one of the main goals of the military health care organizations. This study was aimed to evaluate the service quality of selected military hospitals in Iran based on the Joint Commission International (JCI) standards and comparing these hospitals with each other and ranking them using the analytic hierarchy process (AHP) technique in 2013. This was a cross-sectional and descriptive study conducted on five military hospitals, selected using the purposive sampling method, in 2013. Required data collected using checklists of accreditation standards and nominal group technique. AHP technique was used for prioritizing. Furthermore, Expert Choice 11.0 was used to analyze the collected data. Among JCI standards, the standards of access to care and continuity of care (weight = 0.122), quality improvement and patient safety (weight = 0.121) and leadership and management (weight = 0.117) had the greatest importance, respectively. Furthermore, in the overall ranking, BGT (weight = 0.369), IHM (0.238), SAU (0.202), IHK (weight = 0.125) and SAB (weight = 0.066) ranked first to fifth, respectively. AHP is an appropriate technique for measuring the overall performance of hospitals and their quality of services. It is a holistic approach that takes all hospital processes into consideration. The results of the present study can be used to improve hospitals performance through identifying areas, which are in need of focus for quality improvement and selecting strategies to improve service quality.

Standardization of reagents and methods used in cytological and histological practice with emphasis on dyes, stains and chromogenic reagents

DEFF Research Database (Denmark)

Lyon, H O; De Leenheer, A P; Horobin, R W

1994-01-01

and stains through the preparation of reference materials and the development of chromatographic methods. An overview is presented of the problems concerned with standardization of the Romanowsky-Giemsa stain for cytological and histological application. Finally, the problem of how to convince routine dye...

Systematic evaluation of commercially available ultra-high performance liquid chromatography columns for drug metabolite profiling: optimization of chromatographic peak capacity.

Science.gov (United States)

Dubbelman, Anne-Charlotte; Cuyckens, Filip; Dillen, Lieve; Gross, Gerhard; Hankemeier, Thomas; Vreeken, Rob J

2014-12-29

The present study investigated the practical use of modern ultra-high performance liquid chromatography (UHPLC) separation techniques for drug metabolite profiling, aiming to develop a widely applicable, high-throughput, easy-to-use chromatographic method, with a high chromatographic resolution to accommodate simultaneous qualitative and quantitative analysis of small-molecule drugs and metabolites in biological matrices. To this end, first the UHPLC system volume and variance were evaluated. Then, a mixture of 17 drugs and various metabolites (molecular mass of 151-749Da, logP of -1.04 to 6.7), was injected on six sub-2μm particle columns. Five newest generation core shell technology columns were compared and tested against one column packed with porous particles. Two aqueous (pH 2.7 and 6.8) and two organic mobile phases were evaluated, first with the same flow and temperature and subsequently at each column's individual limit of temperature and pressure. The results demonstrated that pre-column dead volume had negligible influence on the peak capacity and shape. In contrast, a decrease in post-column volume of 57% resulted in a substantial (47%) increase in median peak capacity and significantly improved peak shape. When the various combinations of stationary and mobile phases were used at the same flow rate (0.5mL/min) and temperature (45°C), limited differences were observed between the median peak capacities, with a maximum of 26%. At higher flow though (up to 0.9mL/min), a maximum difference of almost 40% in median peak capacity was found between columns. The finally selected combination of solid-core particle column and mobile phase composition was chosen for its selectivity, peak capacity, wide applicability and peak shape. The developed method was applied to rat hepatocyte samples incubated with the drug buspirone and demonstrated to provide a similar chromatographic resolution, but a 6 times higher signal-to-noise ratio than a more traditional UHPLC

Possibilities and limitations of fast temperature programming as a route towards fast GC

NARCIS (Netherlands)

Deursen, van M.M.; Beens, J.; Cramers, C.A.M.G.; Janssen, J.G.M.

1999-01-01

One possible way to speed up a gas chromatographic analysis is the application of fast temperature programming by using resistive heating techniques. With this heating technique programming rates up to 20° per second can be reached. A relative standard deviation of retention times better than 0.2%

Comparison of core-shell and totally porous ultra high performance liquid chromatographic stationary phases based on their selectivity towards alfuzosin compounds.

Science.gov (United States)

Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

2014-06-13

This paper focuses on the application of a column classification system based on the Katholieke Universiteit Leuven for the characterization of physicochemical properties of core-shell and ultra-high performance liquid chromatographic stationary phases, followed by the verification of the reliability of the obtained column classification in pharmaceutical practice. In the study, 7 stationary phases produced in core-shell technology and 18 ultra-high performance liquid chromatographic columns were chromatographically tested, and ranking lists were built on the FKUL-values calculated against two selected reference columns. In the column performance test, an analysis of alfuzosin in the presence of related substances was carried out using the brands of the stationary phases with the highest ranking positions. Next, a system suitability test as described by the European Pharmacopoeia monograph was performed. Moreover, a study was also performed to achieve a purposeful shortening of the analysis time of the compounds of interest using the selected stationary phases. Finally, it was checked whether methods using core-shell and ultra-high performance liquid chromatographic columns can be an interesting alternative to the high-performance liquid chromatographic method for the analysis of alfuzosin in pharmaceutical practice. Copyright © 2014 Elsevier B.V. All rights reserved.

New method for evaluating irreversible adsorption and stationary phase bleed in gas chromatographic capillary columns.

Science.gov (United States)

Wright, Bob W; Wright, Cherylyn W

2012-10-26

A novel method is described for the evaluation of irreversible adsorption and column bleed in gas chromatographic (GC) columns using a tandem GC approach. This work specifically determined the degree of irreversible adsorption behavior of specific sulfur and phosphorous containing test probe compounds at levels ranging from approximately 50 picograms (pg) to 1 nanogram (ng) on selected gas chromatographic columns. This method does not replace existing evaluation methods that characterize reversible adsorption but provides an additional tool. The test compounds were selected due to their ease of adsorption and their importance in the specific trace analytical detection methodology being developed. Replicate chromatographic columns with 5% phenylmethylpolysiloxane (PMS), polyethylene glycol (wax), trifluoropropylpolysiloxane (TFP), or 78% cyanopropylpolysiloxane stationary phases from a variety of vendors were evaluated. As expected, the results demonstrate that the different chromatographic phases exhibit differing degrees of irreversible adsorption behavior. The results also indicate that all manufacturers do not produce equally inert columns nor are columns from a given manufacturer identical. The wax-coated columns for the test probes used were more inert as a group than 5% PMS coated columns, and they were more reproducibly manufactured. Both TFP and 78% cyanopropylpolysiloxane columns displayed superior inertness to the test compounds compared to either 5% PMS- or wax-coated columns. Irreversible adsorption behavior was characterized for a limited range of stationary phase film thicknesses. In addition, the method was shown effective for characterizing column bleed and methods to remove bleed components. This method is useful in screening columns for demanding applications and to obtain diagnostic information related to improved preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Evaluation of the suitability of chromatographic systems to predict human skin permeation of neutral compounds.

Science.gov (United States)

Hidalgo-Rodríguez, Marta; Soriano-Meseguer, Sara; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

2013-12-18

Several chromatographic systems (three systems of high-performance liquid chromatography and two micellar electrokinetic chromatography systems) besides the reference octanol-water partition system are evaluated by a systematic procedure previously proposed in order to know their ability to model human skin permeation. The precision achieved when skin-water permeability coefficients are correlated against chromatographic retention factors is predicted within the framework of the solvation parameter model. It consists in estimating the contribution of error due to the biological and chromatographic data, as well as the error coming from the dissimilarity between the human skin permeation and the chromatographic systems. Both predictions and experimental tests show that all correlations are greatly affected by the considerable uncertainty of the skin permeability data and the error associated to the dissimilarity between the systems. Correlations with much better predictive abilities are achieved when the volume of the solute is used as additional variable, which illustrates the main roles of both lipophilicity and size of the solute to penetrate through the skin. In this way, the considered systems are able to give precise estimations of human skin permeability coefficients. In particular, the HPLC systems with common C18 columns provide the best performances in emulating the permeation of neutral compounds from aqueous solution through the human skin. As a result, a methodology based on easy, fast, and economical HPLC measurements in a common C18 column has been developed. After a validation based on training and test sets, the method has been applied with good results to the estimation of skin permeation of several hormones and pesticides. Copyright © 2013 Elsevier B.V. All rights reserved.

High-Order Approximation of Chromatographic Models using a Nodal Discontinuous Galerkin Approach

DEFF Research Database (Denmark)

Meyer, Kristian; Huusom, Jakob Kjøbsted; Abildskov, Jens

2018-01-01

by Javeed et al. (2011a,b, 2013) with an efficient quadrature-free implementation. The framework is used to simulate linear and non-linear multicomponent chromatographic systems. The results confirm arbitrary high-order accuracy and demonstrate the potential for accuracy and speed-up gains obtainable...

Principal coordinate analysis assisted chromatographic analysis of bacterial cell wall collection: A robust classification approach.

Science.gov (United States)

Kumar, Keshav; Cava, Felipe

2018-04-10

In the present work, Principal coordinate analysis (PCoA) is introduced to develop a robust model to classify the chromatographic data sets of peptidoglycan sample. PcoA captures the heterogeneity present in the data sets by using the dissimilarity matrix as input. Thus, in principle, it can even capture the subtle differences in the bacterial peptidoglycan composition and can provide a more robust and fast approach for classifying the bacterial collection and identifying the novel cell wall targets for further biological and clinical studies. The utility of the proposed approach is successfully demonstrated by analysing the two different kind of bacterial collections. The first set comprised of peptidoglycan sample belonging to different subclasses of Alphaproteobacteria. Whereas, the second set that is relatively more intricate for the chemometric analysis consist of different wild type Vibrio Cholerae and its mutants having subtle differences in their peptidoglycan composition. The present work clearly proposes a useful approach that can classify the chromatographic data sets of chromatographic peptidoglycan samples having subtle differences. Furthermore, present work clearly suggest that PCoA can be a method of choice in any data analysis workflow. Copyright © 2018 Elsevier Inc. All rights reserved.

Batch-to-batch quality consistency evaluation of botanical drug products using multivariate statistical analysis of the chromatographic fingerprint.

Science.gov (United States)

Xiong, Haoshu; Yu, Lawrence X; Qu, Haibin

2013-06-01

Botanical drug products have batch-to-batch quality variability due to botanical raw materials and the current manufacturing process. The rational evaluation and control of product quality consistency are essential to ensure the efficacy and safety. Chromatographic fingerprinting is an important and widely used tool to characterize the chemical composition of botanical drug products. Multivariate statistical analysis has showed its efficacy and applicability in the quality evaluation of many kinds of industrial products. In this paper, the combined use of multivariate statistical analysis and chromatographic fingerprinting is presented here to evaluate batch-to-batch quality consistency of botanical drug products. A typical botanical drug product in China, Shenmai injection, was selected as the example to demonstrate the feasibility of this approach. The high-performance liquid chromatographic fingerprint data of historical batches were collected from a traditional Chinese medicine manufacturing factory. Characteristic peaks were weighted by their variability among production batches. A principal component analysis model was established after outliers were modified or removed. Multivariate (Hotelling T(2) and DModX) control charts were finally successfully applied to evaluate the quality consistency. The results suggest useful applications for a combination of multivariate statistical analysis with chromatographic fingerprinting in batch-to-batch quality consistency evaluation for the manufacture of botanical drug products.

Chromatographic enrichment of isotopes in hydrogen and water samples on palladium

International Nuclear Information System (INIS)

Andreev, B.M.; Polevoi, A.S.; Perevezentsev, A.N.

1987-01-01

Data on the isotopic enrichment of hydrogen and water samples by chromatography on palladium have been analyzed. Experimental data on the effect of temperature, hydrogen flow, volume of the enriched fraction, and length of the chromatographic column on the degree of separation attainable in the column have been obtained. It has been shown that the maximum separation achievable (regardless of the type of the isotope mixture) at 273 K falls with increase of hydrogen flow and volume of the enriched gas fraction recoverable from the column. A separation degree of ∼ 1040 has been achieved for a mixture of protium and deuterium in a 10-mm wide and 0.6-m long chromatographic column packed with palladium black with a grain size of 0.2-0.5 mm at 273 K and a specific hydrogen flow of 1.22 mole/m 2 x sec. For a protium-tritium mixture a separation degree of ∼ 90 has been reached in a similar column at 273 K and a specific hydrogen flow of 0.4 mole/m 2 x sec

Current Applications of Chromatographic Methods in the Study of Human Body Fluids for Diagnosing Disorders.

Science.gov (United States)

Jóźwik, Jagoda; Kałużna-Czaplińska, Joanna

2016-01-01

Currently, analysis of various human body fluids is one of the most essential and promising approaches to enable the discovery of biomarkers or pathophysiological mechanisms for disorders and diseases. Analysis of these fluids is challenging due to their complex composition and unique characteristics. Development of new analytical methods in this field has made it possible to analyze body fluids with higher selectivity, sensitivity, and precision. The composition and concentration of analytes in body fluids are most often determined by chromatography-based techniques. There is no doubt that proper use of knowledge that comes from a better understanding of the role of body fluids requires the cooperation of scientists of diverse specializations, including analytical chemists, biologists, and physicians. This article summarizes current knowledge about the application of different chromatographic methods in analyses of a wide range of compounds in human body fluids in order to diagnose certain diseases and disorders.

Novel chromatographic separation and carbon solid-phase extraction of acetanilide herbicide degradation products.

Science.gov (United States)

Shoemaker, Jody A

2002-01-01

One acetamide and 5 acetanilide herbicides are currently registered for use in the United States. Over the past several years, ethanesulfonic acid (ESA) and oxanilic acid (OA) degradation products of these acetanilide/acetamide herbicides have been found in U.S. ground waters and surface waters. Alachlor ESA and other acetanilide degradation products are listed on the U.S. Environmental Protection Agency's (EPA) 1998 Drinking Water Contaminant Candidate List. Consequently, EPA is interested in obtaining national occurrence data for these contaminants in drinking water. EPA currently does not have a method for determining these acetanilide degradation products in drinking water; therefore, a research method is being developed using liquid chromatography/negative ion electrospray/mass spectrometry with solid-phase extraction (SPE). A novel chromatographic separation of the acetochlor/alachlor ESA and OA structural isomers was developed which uses an ammonium acetate-methanol gradient combined with heating the analytical column to 70 degrees C. Twelve acetanilide degradates were extracted by SPE from 100 mL water samples using carbon cartridges with mean recoveries >90% and relative standard deviations < or =16%.

Development of new process network for gas chromatograph and analyzers connected with SCADA system and Digital Control Computers at Cernavoda NPP Unit 1

International Nuclear Information System (INIS)

Deneanu, Cornel; Popa Nemoiu, Dragos; Nica, Dana; Bucur, Cosmin

2007-01-01

The continuous monitoring of gas mixture concentrations (deuterium/ hydrogen/oxygen/nitrogen) accumulated in 'Moderator Cover Gas', 'Liquid Control Zone' and 'Heat Transport D 2 O Storage Tank Cover Gas', as well as the continuous monitoring of Heavy Water into Light Water concentration in 'Boilers Steam', 'Boilers Blown Down', 'Moderator heat exchangers', and 'Recirculated Water System', sensing any leaks of Cernavoda NPP U1 led to requirement of developing a new process network for gas chromatograph and analyzers connected to the SCADA system and Digital Control Computers of Cernavoda NPP Unit 1. In 2005 it was designed and implemented the process network for gas chromatograph which connected the gas chromatograph equipment to the SCADA system and Digital Control Computers of the Cernavoda NPP Unit 1. Later this process network for gas chromatograph has been extended to connect the AE13 and AE14 Fourier Transform Infrared (FTIR) analyzers with either. The Gas Chromatograph equipment measures with best accuracy the mixture gases (deuterium/ hydrogen/oxygen/nitrogen) concentration. The Fourier Transform Infrared (FTIR) AE13 and AE14 Analyzers measure the Heavy Water into Light Water concentration in Boilers Steam, Boilers BlownDown, Moderator heat exchangers, and Recirculated Water System, monitoring and signaling any leaks. The Gas Chromatograph equipment and Fourier Transform Infrared (FTIR) AE13 and AE14 Analyzers use the new OPC (Object Link Embedded for Process Control) technologies available in ABB's VistaNet network for interoperability with automation equipment. This new process network has interconnected the ABB chromatograph and Fourier Transform Infrared analyzers with plant Digital Control Computers using new technology. The result was an increased reliability and capability for inspection and improved system safety

Relationship between alveolar bone measured by 125I absorptiometry with analysis of standardized radiographs: 2. Bjorn technique

International Nuclear Information System (INIS)

Ortman, L.F.; McHenry, K.; Hausmann, E.

1982-01-01

The Bjorn technique is widely used in periodontal studies as a standardized measure of alveolar bone. Recent studies have demonstrated the feasibility of using 125 I absorptiometry to measure bone mass. The purpose of this study was to compare 125 I absorptiometry with the Bjorn technique in detecting small sequential losses of alveolary bone. Four periodontal-like defects of incrementally increasing size were produced in alveolar bone in the posterior segment of the maxilla of a human skull. An attempt was made to sequentially reduce the amount of bone in 10% increments until no bone remained, a through and through defect. The bone remaining at each step was measured using 125 I absorptiometry. At each site the 125 I absorptiometry measurements were made at the same location by fixing the photon source to a prefabricated precision-made occlusal splint. This site was just beneath the crest and midway between the borders of two adjacent teeth. Bone loss was also determined by the Bjorn technique. Standardized intraoral films were taken using a custom-fitted acrylic clutch, and bone measurements were made from the root apex to coronal height of the lamina dura. A comparison of the data indicates that: (1) in early bone loss, less than 30%, the Bjorn technique underestimates the amount of loss, and (2) in advanced bone loss, more than 60% the Bjorn technique overestimates it

Application of liquid chromatography techniques to the measurement of soluble transition metals in PWR primary coolant

International Nuclear Information System (INIS)

Amey, M.D.H.; Brown, G.R.

1987-01-01

Two chromatographic techniques have been developed, and evaluated for the on-line analysis of soluble transition metals, particularly cobalt, in PWR primary coolant. Automatic operation and control, together with data processing and storage has been achieved by interfacing a Dionex ion chromatograph to a microprocessor control system. An absolute detection limit of 0.1 ng cobalt has been obtained which, with on-line sample preconcentration (100 ml), has enabled measurements to be made down to part-per-trillion levels (0.001 ppb). Application of the techniques to PWR coolant analysis was demonstrated by a programme of work on the Half Megawatt Loop at Winfrith. During this work some aspects of the behaviour of soluble metal species have been studied in both de-oxygenated and hydrogenated conditions. The effects of changes in coolant chemistry, operating temperature, and sample line flowrates on circulating impurity levels are reported, together with the dramatic effects observed when part of the circuit pipework was replaced with new stainless steel tubing. (author)

Specific binding assay technique; standardization of reagent

International Nuclear Information System (INIS)

Huggins, K.G.; Roitt, I.M.

1979-01-01

The standardization of a labelled constituent, such as anti-IgE, for use in a specific binding assay method is disclosed. A labelled ligand, such as IgE, is standardized against a ligand reference substance, such as WHO standard IgE, to determine the weight of IgE protein represented by the labelled ligand. Anti-light chain antibodies are contacted with varying concentrations of the labelled ligand. The ligand is then contacted with the labelled constituent which is then quantitated in relation to the amount of ligand protein present. The preparation of 131 I-labelled IgE is described. Also disclosed is an improved specific binding assay test method for determining the potency of an allergen extract in serum from an allergic individual. The improvement involved using a parallel model system of a second complex which consisted of anti-light chain antibodies, labelled ligand and the standardized labelled constituent (anti-IgE). The amount of standardized labelled constituent bound to the ligand in the first complex was determined, as described above, and the weight of ligand inhibited by addition of soluble allergen was then used as a measure of the potency of the allergen extract. (author)

A rapid hydrophilic interaction liquid chromatographic determination of glimepiride in pharmaceutical formulations

Directory of Open Access Journals (Sweden)

Si Zhou

2017-09-01

Full Text Available Glimepiride is one of the most widely prescribed antidiabetic drugs and contains both hydrophobic and hydrophilic functional groups in its molecules, and thus could be analyzed by either reversed-phase high performance liquid chromatography (HPLC or hydrophilic interaction liquid chromatography (HILIC. In the literature, however, only reversed-phase HPLC has been reported. In this study, a simple, rapid and accurate hydrophilic interaction liquid chromatographic method was developed for the determination of glimepiride in pharmaceutical formulations. The analytical method comprised a fast ultrasound-assisted extraction with acetonitrile as a solvent followed by HILIC separation and quantification using a Waters Spherisorb S5NH2 hydrophilic column with a mobile phase consisting of acetonitrile and aqueous acetate buffer (5.0 mM. The retention time of glimepiride increased slightly with decrease of mobile phase pH value from 6.8 to 5.8 and of acetonitrile content from 60% to 40%, indicating that both hydrophilic, ionic, and hydrophobic interactions were involved in the HILIC retention and elution mechanisms. Quantitation was carried out with a mobile phase of 40% acetonitrile and 60% aqueous acetate buffer (5.0 mM at pH 6.3, by relating the peak area of glimepiride to that of the internal standard, with a detection limit of 15.0 μg/L. UV light absorption responses at 228 nm were linear over a wide concentration range from 50.0 μg/L to 6.00 mg/L. The recoveries of the standard added to pharmaceutical tablet samples were 99.4–103.0% for glimepiride, and the relative standard deviation for the analyte was less than 1.0%. This method has been successfully applied to determine the glimepiride contents in pharmaceutical formulations.

Derivatization reactions in the gas—liquid chromatographic analysis of drugs in biological fluids

NARCIS (Netherlands)

Hulshoff, A.; Lingeman, H.

1984-01-01

Alkylation, acylation, silylation and other derivatization reactions applied to the gas chromatographic analysis of drugs in biological matrices are reviewed. Reaction conditions are discussed in relation to reaction mechanisms. Detector-oriented labelling of drugs, and derivatization with chiral

Automation of an ion chromatograph for precipitation analysis with computerized data reduction

Science.gov (United States)

Hedley, Arthur G.; Fishman, Marvin J.

1982-01-01

Interconnection of an ion chromatograph, an autosampler, and a computing integrator to form an analytical system for simultaneous determination of fluoride, chloride, orthophosphate, bromide, nitrate, and sulfate in precipitation samples is described. Computer programs provided with the integrator are modified to implement ionchromatographic data reduction and data storage. The liquid-flow scheme for the ion chromatograph is changed by addition of a second suppressor column for greater analytical capacity. An additional vave enables selection of either suppressor column for analysis, as the other column is regenerated and stabilized with concentrated eluent.Minimum limits of detection and quantitation for each anion are calculated; these limits are a function of suppressor exhaustion. Precision for replicate analyses of six precipitation samples for fluoride, chloride, orthophosphate, nitrate, and sulfate ranged from 0.003 to 0.027 milligrams per liter. To determine accuracy of results, the same samples were spiked with known concentrations of the above mentioned anions. Average recovery was 108 percent.

Porous Chromatographic Materials as Substrates for Preparing Synthetic Nuclear Explosion Debris Particles

International Nuclear Information System (INIS)

Harvey, Scott D.; Liezers, Martin; Antolick, Kathryn C.; Garcia, Ben J.; Sweet, Lucas E.; Carman, April J.; Eiden, Gregory C.

2013-01-01

In this study, we investigated several porous chromatographic materials as synthetic substrates for preparing surrogate nuclear explosion debris particles. The resulting synthetic debris materials are of interest for use in developing analytical methods. Eighteen metals, including some of forensic interest, were loaded onto materials by immersing them in metal solutions (556 mg/L of each metal) to fill the pores, applying gentle heat (110°C) to drive off water, and then treating them at high temperatures (up to 800°C) in air to form less soluble metal species. High-boiling-point metals were uniformly loaded on spherical controlled-pore glass to emulate early fallout, whereas low-boiling-point metals were loaded on core-shell silica to represent coated particles formed later in the nuclear fallout-formation process. Analytical studies were applied to characterize solubility, material balance, and formation of recalcitrant species. Dissolution experiments indicated loading was 1.5 to 3 times higher than expected from the pore volume alone, a result attributed to surface coating. Analysis of load solutions before and after filling the material pores revealed that most metals were passively loaded; that is, solutions filled the pores without active metal discrimination. However, niobium and tin concentrations were lower in solutions after pore filling, and were found in elevated concentrations in the final products, indicating some metals were selectively loaded. High-temperature treatments caused reduced solubility of several metal species, and loss of some metals (rhenium and tellurium) because volatile species were formed. Sample preparation reproducibility was high (the inter-batch relative standard deviation was 7.8%, and the intra-batch relative standard deviation was 0.84%) indicating that this material is suitable for use as a working standard for analytical methods development. We anticipate future standardized radionuclide-loaded materials will find use in

Automated chromatographic laccase-mediator-system activity assay.

Science.gov (United States)

Anders, Nico; Schelden, Maximilian; Roth, Simon; Spiess, Antje C

2017-08-01

To study the interaction of laccases, mediators, and substrates in laccase-mediator systems (LMS), an on-line measurement was developed using high performance anion exchange chromatography equipped with a CarboPac™ PA 100 column coupled to pulsed amperometric detection (HPAEC-PAD). The developed method was optimized for overall chromatographic run time (45 to 120 min) and automated sample drawing. As an example, the Trametes versicolor laccase induced oxidation of 1-(3,4-dimethoxyphenyl)-2-(2-methoxyphenoxy)-1,3-dihydroxypropane (adlerol) using 1-hydroxybenzotriazole (HBT) as mediator was measured and analyzed on-line. Since the Au electrode of the PAD detects only hydroxyl group containing substances with a limit of detection being in the milligram/liter range, not all products are measureable. Therefore, this method was applied for the quantification of adlerol, and-based on adlerol conversion-for the quantification of the LMS activity at a specific T. versicolor laccase/HBT ratio. The automated chromatographic activity assay allowed for a defined reaction start of all laccase-mediator-system reactions mixtures, and the LMS reaction progress was automatically monitored for 48 h. The automatization enabled an integrated monitoring overnight and over-weekend and minimized all manual errors such as pipetting of solutions accordingly. The activity of the LMS based on adlerol consumption was determined to 0.47 U/mg protein for a laccase/mediator ratio of 1.75 U laccase/g HBT. In the future, the automated method will allow for a fast screening of combinations of laccases, mediators, and substrates which are efficient for lignin modification. In particular, it allows for a fast and easy quantification of the oxidizing activity of an LMS on a lignin-related substrate which is not covered by typical colorimetric laccase assays. ᅟ.

Ion Chromatographic Method with Post-Column Fuchsin Reaction for Measurement of Bromate in Chlorinated Water

Directory of Open Access Journals (Sweden)

Homer C. Genuino

2009-06-01

Full Text Available An ion chromatographic method that employs a post-column reaction with fuchsin and spectrophotometric detection was optimized for measuring bromate (BrO3- in water. BrO3- is converted to Br2 by sodium metabisulfite and then reacted with acidic fuchsin to form a red-colored product that strongly absorbs at 530 nm. The reaction of BrO3- and fuchsin reagent is optimum at pH 3.5 and 65 oC. The method has a limit of quantitation of 4.5 µg L-1 and is linear up to 150 µg L-1 BrO3-. Recoveries from spiked samples were high ranging from 95 to 102 % using external standard calibration and 87 to 103 % using standard addition method. Intra-batch and inter-batch reproducibility studies of the method resulted to RSD values ranging from 0.62 to 2.01 % and percent relative error of 0.12 to 2.94 % for BrO3- concentrations of 10 µg L-1 and 50 µg L-1. This method is free of interferences from common inorganic anions at levels typically found in chlorinated tap drinking water without preconcentration. The optimized method can be applied to trace analysis of bromate in chlorinated tap drinking water samples.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

Science.gov (United States)

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Modeling chromatographic columns. Non-equilibrium packed-bed adsorption with non-linear adsorption isotherms

NARCIS (Netherlands)

Özdural, A.R.; Alkan, A.; Kerkhof, P.J.A.M.

2004-01-01

In this work a new mathematical model, based on non-equilibrium conditions, describing the dynamic adsorption of proteins in columns packed with spherical adsorbent particles is used to study the performance of chromatographic systems. Simulations of frontal chromatography, including axial

Fluorescent quenching immune chromatographic strips with quantum dots and upconversion nanoparticles as fluorescent donors for visual detection of sulfaquinoxaline in foods of animal origin

International Nuclear Information System (INIS)

Hu, Gaoshuang; Sheng, Wei; Li, Jingmin; Zhang, Yan; Wang, Junping; Wang, Shuo

2017-01-01

In this study, two novel fluorescence quenching immune chromatographic strips (FQICS) were developed to detect sulfaquinoxaline (SQX) in foods of animal origin. These proposed FQICSs were based on fluorescence resonance energy transfer (FRET) from fluorescence donors (quantum dots or upconversion nanoparticles) to fluorescence acceptors (colloidal gold nanoparticles). Compared with traditional colloidal gold-based immune chromatographic strips (ICS), these FQICSs showed positive correlation between the fluorescent signals and the targets, and allowed user to get test results from weak fluorescent signals. The visual detection limits of these two FQICSs were both 1 ng mL −1 in standard solution and 8 μg kg −1 in samples, while the visual detection limit of the colloidal gold-based ICS was 10 ng mL −1 in standard solution and 80 μg kg −1 in samples. Besides, the results we obtained by the use of FQICS showed high agreement with those obtained by the use of commercial ELISA kits, indicating the good accuracy of these strips. As a conclusion, these proposed FQICS based on quantum dots and upconversion nanoparticles can be applied in sensitive, rapid and on-site detection of SQX in foods of animal origin. - Highlights: • Two novel FQICS based on FRET were developed for the first time. • QDs and UCNPs were used as fluorescent donors in the FQICS. • The proposed FQICS showed low LOD compared with traditional ICS. • The proposed FQICS were applied in real samples analysis. • The proposed FQICS were verified by commercial ELISA kits.

MIMO wireless networks channels, techniques and standards for multi-antenna, multi-user and multi-cell systems

CERN Document Server

Clerckx, Bruno

2013-01-01

This book is unique in presenting channels, techniques and standards for the next generation of MIMO wireless networks. Through a unified framework, it emphasizes how propagation mechanisms impact the system performance under realistic power constraints. Combining a solid mathematical analysis with a physical and intuitive approach to space-time signal processing, the book progressively derives innovative designs for space-time coding and precoding as well as multi-user and multi-cell techniques, taking into consideration that MIMO channels are often far from ideal. Reflecting developments

Bioanalytical HPTLC Method for Estimation of Zolpidem Tartrate from Human Plasma

OpenAIRE

Abhay R. Shirode; Bharti G. Jadhav; Vilasrao J. Kadam

2016-01-01

A simple and selective high performance thin layer chromatographic (HPTLC) method was developed and validated for the estimation of zolpidem tartrate from human plasma using eperisone hydrochloride as an internal standard (IS). Analyte and IS were extracted from human plasma by liquid liquid extraction (LLE) technique. The Camag HPTLC system, employed with software winCATS (ver.1.4.1.8) was used for the proposed bioanalytical work. Planar chromatographic development was carried out with the h...

The chromatographic behavior of arsenic compounds on anion exchange columns with binary organic acids as mobile phases

Energy Technology Data Exchange (ETDEWEB)

Zheng, J.; Goessler, W.; Kosmus, W. [Graz Univ. (Austria). Inst. fuer Analytische Chemie

1998-03-01

Identification and quantification of arsenic compounds was performed with high-performance liquid chromatography (HPLC) and flame atomic absorption spectrometry (FAAS) as element-specific detector. Arsenous acid, methylarsonic acid, dimethylarsinic acid, arsenic acid, arsenobetaine, and arsenocholine were separated on two anion-exchange columns (Synchropak Q 300 and PRP-X 100) with different binary organic acids as mobile phases. The influence of chromatographic parameters, such as pH and the concentration of the mobile phase were investigated. An unusual chromatographic behavior of arsenous acid was observed when tartaric acid was used as mobile phase. (orig.)

Improved stochastic resonance algorithm for enhancement of signal-to-noise ratio of high-performance liquid chromatographic signal

International Nuclear Information System (INIS)

Xie Shaofei; Xiang Bingren; Deng Haishan; Xiang Suyun; Lu Jun

2007-01-01

Based on the theory of stochastic resonance, an improved stochastic resonance algorithm with a new criterion for optimizing system parameters to enhance signal-to-noise ratio (SNR) of HPLC/UV chromatographic signal for trace analysis was presented in this study. Compared with the conventional criterion in stochastic resonance, the proposed one can ensure satisfactory SNR as well as good peak shape of chromatographic peak in output signal. Application of the criterion to experimental weak signals of HPLC/UV was investigated and the results showed an excellent quantitative relationship between different concentrations and responses

High performance liquid chromatographic determination of glucosamine in rat plasma.

Science.gov (United States)

Aghazadeh-Habashi, Ali; Sattari, Saeed; Pasutto, Franco; Jamali, Fakhreddin

2002-01-01

A high performance liquid chromatographic method was developed for the determination of glucosamine (GlcN) in rat plasma. Internal standard, galactosamine, was added to 100 micro L of plasma containing GlcN followed by precipitation of plasma proteins with acetonitrile. Evaporation of the decanted supernatant solution was accelerated by the addition of methanol. GlcN was derivatized by addition of a solution containing 1-naphthyl isothiocyanate. Sample cleanup included passage through an anion exchange cartridge. Analysis was accomplished by injection of 0.1 mL of the sample solution into an isocratic HPLC system consisting of a C18 column, a mobile phase of acetonitrile: water: acetic acid: triethylamine (4.5: 95.5:0.1:0.05), a flow rate of 0.9 mL/min, and a UV detector set at 254 nm. Galactosamine and GlcN appeared 26 and 29 min post-injection, respectively. The assay was linear over the range of 1.25-400 micro g/mL (CV<10%) with a detection limit of 0.63 microg/mL and a limit of quantification of 1.25 microg/mL. The method was applied to the determination of GlcN in rat plasma after oral administration of 350 mg/kg of GlcN hydrochloride. The present assay is specific, sensitive, precise, and accurate and is suitable for pharmacokinetic studies.

PROCAL: A Set of 40 Peptide Standards for Retention Time Indexing, Column Performance Monitoring, and Collision Energy Calibration.

Science.gov (United States)

Zolg, Daniel Paul; Wilhelm, Mathias; Yu, Peng; Knaute, Tobias; Zerweck, Johannes; Wenschuh, Holger; Reimer, Ulf; Schnatbaum, Karsten; Kuster, Bernhard

2017-11-01

Beyond specific applications, such as the relative or absolute quantification of peptides in targeted proteomic experiments, synthetic spike-in peptides are not yet systematically used as internal standards in bottom-up proteomics. A number of retention time standards have been reported that enable chromatographic aligning of multiple LC-MS/MS experiments. However, only few peptides are typically included in such sets limiting the analytical parameters that can be monitored. Here, we describe PROCAL (ProteomeTools Calibration Standard), a set of 40 synthetic peptides that span the entire hydrophobicity range of tryptic digests, enabling not only accurate determination of retention time indices but also monitoring of chromatographic separation performance over time. The fragmentation characteristics of the peptides can also be used to calibrate and compare collision energies between mass spectrometers. The sequences of all selected peptides do not occur in any natural protein, thus eliminating the need for stable isotope labeling. We anticipate that this set of peptides will be useful for multiple purposes in individual laboratories but also aiding the transfer of data acquisition and analysis methods between laboratories, notably the use of spectral libraries. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Test plan for demonstrating plutonium extraction from 10-L solutions using EIChrom extraction chromatographic resins

International Nuclear Information System (INIS)

Barney, G.S.

1994-01-01

Corrosive plutonium solutions stored in 10-L containers at the Plutonium Finishing Plant must be treated to convert the plutonium to a safe, solid form for storage and to remove the americium so that radiation exposure can be reduced. Extraction chromatographic resins will be tested for separating plutonium from these solutions in the laboratory. Separation parameters will be developed during the testing for large scale processing of the 10-L solutions and solutions of similar composition. Use of chromatographic resins will allow plutonium separation with minimum of chemical addition to the feed and without the need for plutonium valence adjustment. The separated plutonium will be calcined to plutonium oxide by direct solution calcination

Comparative Studies on the Radiolabeling and Chromatographic Purification of Some Medically Important Compounds

International Nuclear Information System (INIS)

El-Gizawy, M.A.E.

2013-01-01

The present thesis comprises five basic chapters: The first chapter includes the main idea of our study and its problems, also includes the aim of the work of our study. The second chapter includes the theoretical consideration of the subject. It deals with the general methods of labeling, factors that influence the integrity of labeled compounds, radionuclides used for diagnostic nuclear medicine, production methods and radioactive properties of 123 I, 125 I and 131 I. It includes also the techniques used for the preparation of the radioiodinated compounds especially the electrophilic radioiodination technique. This chapter deals also with the medical imaging, techniques of diagnostic nuclear medicine and the purification of radioiodinated compounds using different chromatographic techniques. Since these radioiodinated compounds are used for diagnosis and therapeutic treatment of human diseases, quality control tests such as determination of chemical purity, radionuclidic purity, radiochemical purity, sterility, pyrogenicity and biodistribution are performed to ensure the purity, the safety and efficiency of these products for the intended nuclear medicine application. The third chapter describes the experimental section; comprising chemicals, reagents, the radionuclides, the equipments and the counting systems used in the study. It describes the electrophilic radioiodination using chloramine-T (CAT), iodogen and lactoperoxidase oxidizing agents and the factors affecting the radiochemical yield of the radioiodination of histamine and L-tyrosine methyl ester such as substrate concentration, ph of the medium, reaction time, temperature and stability of the labeled product. This chapter also includes the techniques used in the Purification of radioiodinated compounds, including paper electrophoresis, thin layer chromatography (TLC), Poly acrylamide-acrylic acid resin [P(AAm-AA) resin] and high performance liquid chromatography (HPLC), in addition, the quality control

Warping methods for spectroscopic and chromatographic signal alignment: A tutorial

Energy Technology Data Exchange (ETDEWEB)

Bloemberg, Tom G., E-mail: T.Bloemberg@science.ru.nl [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Radboud University Nijmegen, Education Institute for Molecular Sciences, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Gerretzen, Jan; Lunshof, Anton [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Wehrens, Ron [Centre for Research and Innovation, Fondazione Edmund Mach, Via E. Mach, 1, 38010 San Michele all’Adige, TN (Italy); Buydens, Lutgarde M.C. [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands)

2013-06-05

Highlights: •The concepts of warping and alignment are introduced. •The most important warping methods are critically reviewed and explained. •Reference selection, evaluation and place of warping in preprocessing are discussed. •Some pitfalls, especially for LC–MS and similar data, are addressed. •Examples are provided, together with programming scripts to rework and extend them. -- Abstract: Warping methods are an important class of methods that can correct for misalignments in (a.o.) chemical measurements. Their use in preprocessing of chromatographic, spectroscopic and spectrometric data has grown rapidly over the last decade. This tutorial review aims to give a critical introduction to the most important warping methods, the place of warping in preprocessing and current views on the related matters of reference selection, optimization, and evaluation. Some pitfalls in warping, notably for liquid chromatography–mass spectrometry (LC–MS) data and similar, will be discussed. Examples will be given of the application of a number of freely available warping methods to a nuclear magnetic resonance (NMR) spectroscopic dataset and a chromatographic dataset. As part of the Supporting Information, we provide a number of programming scripts in Matlab and R, allowing the reader to work the extended examples in detail and to reproduce the figures in this paper.

Advanced techniques for energy-efficient industrial-scale continuous chromatography

Energy Technology Data Exchange (ETDEWEB)

DeCarli, J.P. II (Dow Chemical Co., Midland, MI (USA)); Carta, G. (Virginia Univ., Charlottesville, VA (USA). Dept. of Chemical Engineering); Byers, C.H. (Oak Ridge National Lab., TN (USA))

1989-11-01

Continuous annular chromatography (CAC) is a developing technology that allows truly continuous chromatographic separations. Previous work has demonstrated the utility of this technology for the separation of various materials by isocratic elution on a bench scale. Novel applications and improved operation of the process were studied in this work, demonstrating that CAC is a versatile apparatus which is capable of separations at high throughput. Three specific separation systems were investigated. Pilot-scale separations at high loadings were performed using an industrial sugar mixture as an example of scale-up for isocratic separations. Bench-scale experiments of a low concentration metal ion mixture were performed to demonstrate stepwise elution, a chromatographic technique which decreases dilution and increases sorbent capacity. Finally, the separation of mixtures of amino acids by ion exchange was investigated to demonstrate the use of displacement development on the CAC. This technique, which perhaps has the most potential, when applied to the CAC allowed simultaneous separation and concentration of multicomponent mixtures on a continuous basis. Mathematical models were developed to describe the CAC performance and optimize the operating conditions. For all the systems investigated, the continuous separation performance of the CAC was found to be very nearly the same as the batchwise performance of conventional chromatography. the technology appears, thus, to be very promising for industrial applications. 43 figs., 9 tabs.

Current medical research with the application of coupled techniques with mass spectrometry

OpenAIRE

Ka?u?na-Czapli?ska, Joanna

2011-01-01

Summary The most effective methods of analysis of organic compounds in biological fluids are coupled chromatographic techniques. Capillary gas chromatography/mass spectrometry (GC-MS) allows the most efficient separation, identification and quantification of volatile metabolites in biological fluids. Liquid chromatography-mass spectrometry (LC-MS) is especially suitable for the analysis of non-volatile and/or thermally unstable compounds. A major drawback of liquid chromatography-mass spectro...

First measurements of H2O2 and organic peroxide surface fluces by the Relaxed Eddy Accumulation technique

NARCIS (Netherlands)

Valverde-Canossa, J.; Ganzeveld, L.N.; Rappenglück, B.; Steinbrecher, R.; Klemm, O.; Schuster, G.; Moortgat, G.K.

2006-01-01

The relaxed eddy-accumulation (REA) technique was specially adapted to a high-performance liquid chromatographer (enzymatic method) and scrubbing coils to measure concentrations and fluxes of hydrogen peroxide (H2O2) and organic peroxides with a carbon chain C4, of which only methylhydroperoxide

[Research on the application of grey system theory in the pattern recognition for chromatographic fingerprints of traditional Chinese medicine].

Science.gov (United States)

Wei, Hang; Lin, Li; Zhang, Yuan; Wang, Lianjing; Chen, Qinqun

2013-02-01

A model based on grey system theory was proposed for pattern recognition in chromatographic fingerprints (CF) of traditional Chinese medicine (TCM). The grey relational grade among the data series of each testing CF and the ideal CF was obtained by entropy and norm respectively, then the principle of "maximal matching degree" was introduced to make judgments, so as to achieve the purpose of variety identification and quality evaluation. A satisfactory result in the high performance liquid chromatographic (HPLC) analysis of 56 batches of different varieties of Exocarpium Citrus Grandis was achieved with this model. The errors in the chromatographic fingerprint analysis caused by traditional similarity method or grey correlation method were overcome, as the samples of Citrus grandis 'Tomentosa' and Citrus grandis (L.) Osbeck were correctly distinguished in the experiment. Furthermore in the study on the variety identification of Citrus grandis 'Tomentosa', the recognition rates were up to 92.85%, although the types and the contents of the chemical compositions of the samples were very close. At the same time, the model had the merits of low computation complexity and easy operation by computer programming. The research indicated that the grey system theory has good applicability to pattern recognition in the chromatographic fingerprints of TCM.

Application of extraction-chromatographic concentration to atomic absorption determination of lead and cadmium in drinking and sea water

International Nuclear Information System (INIS)

Bol'shova, T.A.; Agapkina, G.I.; Ershova, N.I.; Narankho, K.E.

1988-01-01

To increase the detection limits for lead and cadmium atomic-absorption determination in natural waters methods of extraction-chromatographic concentration of these metals using tri-n-octylamine (TOA) on polytetrafluoroethylene (PTFE) is developed. Chromatograpy was carried out from 1.5-2.0 M HBr solutions. For cadmium and lead elution acetic acid was used. It is shown that extraction-chromatographic concentration permits to decrease limits of metal atomic-absorption detection by 10 3 with the 500 ml volume sample analysis

Chromatographic method of measurement of helium concentration in underground waters for dating in hydrological questions

International Nuclear Information System (INIS)

Najman, J.

2008-04-01

Research methods which use natural environmental indicators are widely applied in hydrology. Different concentrations of indicators and their isotopic components in ground waters allow to determine the genesis of waters and are valuable source of information about the water flow dynamics. One of the significant indicator is helium. The concentration of 4 He (helium) in ground water is a fine indicator in water dating in a range from a hundreds to millions of years (Aeschbach-Hertig i in., 1999; Andrews i in., 1989; Castro i in., 2000; Zuber i in., 2007). 4 He is also used for dating young waters of age about 10 years (Solomon i in., 1996). Thesis consist the description of elaborated in IFJ PAN in Krakow chromatographic measurement method of helium concentration in ground waters in aim of dating. Chapter 1 contain short introduction about ground water dating and chapter 2 description of helium property and chosen applications of helium for example in technology and earthquake predictions. Helium sources in ground waters are described in chapter 3. Helium concentration in water after infiltration (originated from atmosphere) to the ground water system depends mainly on the helium concentration coming from the equilibration with the atmosphere increased by additional concentration from '' excess air ''. With the increasing resistance time of ground water during the flow, radiogenic, non-atmospheric component of helium dissolves also in water. In chapter 4 two measurement methods of helium concentration in ground waters were introduced: mass spectrometric and gas chromatographic method. Detailed description of elaborated chromatographic measurement method of helium concentration in ground water contain chapter 5. To verify developed method the concentration of helium in ground waters from the regions of Krakow and Busko Zdroj were measured. For this waters the concentrations of helium are known from the earlier mass spectrometric measurements. The results of

Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

Science.gov (United States)

Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

2012-05-01

The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

Development of the H-point standard additions method for coupled liquid-chromatography and UV-visible spectrophotometry

Energy Technology Data Exchange (ETDEWEB)

Campins-Falco, Pilar; Bosch-Reig, Francisco; Herraez-Hernandez, Rosa; Sevillano-Cabeza, Adela (Universidad de Valencia (Spain). Facultad de Quimica, Departamento de Quimica Analitica)

1992-02-10

This work establishes the fundamentals of the H-point standard additions method for liquid chromatography for the simultaneous analysis of binary mixtures with overlapped chromatographic peaks. The method was compared with the deconvolution method of peak suppression and the second derivative of elution profiles. Different mixtures of diuretics were satisfactorily resolved. (author). 21 refs.; 9 figs.; 2 tabs.

Mass fragmentographic analysis of total cholesterol in serum using a heptadeuterated internal standard

International Nuclear Information System (INIS)

Wolthers, B.G.; Hindriks, F.R.; Muskiet, F.A.J.; Groen, A.

1980-01-01

A mass fragmentographic method for the determination of total cholesterol in serum using heptadeuterated [25,26,26,26,27,27,27- 2 H] cholesterol as internal standard is presented. The results obtained are compared with a colorimetric and gas chromatographic method which were previously proposed as reference methods. Criteria for the development of absolute measurement by means of mass fragmentography and stable isotopically labelled internal standards are given. The conclusion is drawn that, at present, mass fragmentographic methods for the determination of total cholesterol in serum do not fulfil the criteria required for absolute methods. (Auth.)

Automated-process gas-chromatograph system for use in accelerated corrosion testing of HTGR core-support posts

International Nuclear Information System (INIS)

Harper, R.E.; Herndon, P.G.

1982-01-01

An automated-process gas chromatograph is the heart of a gaseous-impurities-analysis system developed for the Oak Ridge National Laboratory Core Support Performance Test, at which graphite core-support posts for high-temperature gas-cooled fission reactors are being subjected to accelerated corrosion tests under tightly controlled conditions of atmosphere and temperature. Realistic estimation of in-core corrosion rates is critically dependent upon the accurate measurement of low concentrations of CO, CO 2 , CH 4 , H 2 , and O 2 in the predominantly helium atmosphere. In addition, the capital and labor investment associated with each test puts a premium upon the reliability of the analytical system, as excessive downtime or failure to obtain accurate data would result in unacceptable costs and schedule delays. After an extensive survey of available measurement techniques, gas chromatography was chosen for reasons of accuracy, flexibility, good-performance record, and cost

Review of UV spectroscopic, chromatographic, and electrophoretic methods for the cholinesterase reactivating antidote pralidoxime (2-PAM).

Science.gov (United States)

John, Harald; Blum, Marc-Michael

2012-01-01

Pralidoxime (2-PAM) belongs to the class of monopyridinium oximes with reactivating potency on cholinesterases inhibited by phosphylating organophosphorus compounds (OPC), for example, pesticides and nerve agents. 2-PAM represents an established antidote for the therapy of anticholinesterase poisoning since the late 1950s. Quite high therapeutic concentrations in human plasma (about 13 µg/ml) lead to concentrations in urine being about 100 times higher allowing the use of less sensitive analytical techniques that were used especially in the early years after 2-PAM was introduced. In this time (mid-1950s until the end of the 1970s) 2-PAM was most often analyzed by either paper chromatography or simple UV spectroscopic techniques omitting any sample separation step. These methods were displaced completely after the establishment of column liquid chromatography in the early 1980s. Since then, diverse techniques including cation exchange, size-exclusion, reversed-phase, and ligand-exchange chromatography have been introduced. Today, the most popular method for 2-PAM quantification is ion pair chromatography often combined with UV detection representing more than 50% of all column chromatographic procedures published. Furthermore, electrophoretic approaches by paper and capillary zone electrophoresis have been successfully used but are seldom applied. This review provides a commentary and exhaustive summary of analytical techniques applied to detect 2-PAM in pharmaceutical formulations and biological samples to characterize stability and pharmacokinetics as well as decomposition and biotransformation products. Separation techniques as well as diverse detectors are discussed in appropriate detail allowing comparison of individual preferences and limitations. In addition, novel data on mass spectrometric fragmentation of 2-PAM are provided. Copyright © 2011 John Wiley & Sons, Ltd.

Chromatographic retention and structure roofing tile effect of isomers and its fine structure

NARCIS (Netherlands)

Walraven, J.J.; Ladon, A.W.; Keulemans, A.I.M.

1968-01-01

Logarithmic plots of gas chromatographic retention data for different classes of compds. on different pairs of stationary phases were constructed. A remarkable effect was found. Isomers are spread along parallel lines in a repeated pattern, forming a \\"roofing-tile\\" series. The scattering of points

Green Chromatographic Separation of Coumarin and Vanillins Using Subcritical Water as the Mobile Phase.

Science.gov (United States)

Kayan, Berkant; Akay, Sema; Yang, Yu

2016-08-01

Pure water was used as the eluent for separation of coumarin, vanillin and ethyl vanillin at temperatures ranging from 100 to 200°C using a homemade subcritical water chromatography (SBWC) system. Chromatographic separations were performed on five commercial columns including XTerra MS C18, XBridge C18, Zorbax RRHD Eclipse Plus, Zorbax SB-Phenyl and Zorbax SB-C18 columns. The retention time of all three solutes decreased with increasing water temperature. The shortest retention time among all acceptable separations, less than 4 min, was achieved on the Zorbax SB-C18 column at 200°C. While separations on the XTerra MS C18 column resulted in fronting peaks and a degradation peak from ethyl vanillin on the Zorbax RRHD Eclipse Plus column was observed, all three other columns yielded reasonable separations under SBWC conditions. In addition to separation of the standard test mixture, separation of coumarin contained in a skincare cream sample was also carried out using SBWC. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Gas chromatographic determination with electron capture detection of residual ethylene oxide in intraocular lenses

Energy Technology Data Exchange (ETDEWEB)

Kikuchi, H.; Nakamura, A.; Tsuji, K.

1988-01-01

A sensitive method is described to determine trace quantities of ethylene oxide (EO) in EO-sterilized intraocular lenses (IOLs). An IOL is dipped in ethanol containing 0.25 ppm propylene oxide (PO) in a 4 mL vial, 2 drops of freshly distilled hydrobromic acid is added through a septum, and the mixture is warmed at 50/sup 0/C for 24 h. It is then neutralized by vigorous shaking with sodium bicarbonate, dehydrated with anhydrous sodium sulfate, and filtered. The filtrate is injected into a gas chromatograph with electron-capture detection, and the peak height ratio of ethylene bromohydrin/propylene bromohydrin is measured. EO residue is calculated from the calibration curve obtained through a similar procedure with the standard EO/PO solutions. The limit of determination is 0.04 ..mu..g/lens (ca 2.0 ppm). When EO residue levels were determined for IOLs sampled at 3 different aeration periods after stabilization, the authors found that 9 days of aeration was necessary to meet the US Food and Drug Administration proposed limit for EO residue in IOLs.

Evaluation of chromatographic columns packed with semi- and fully porous particles for benzimidazoles separation.

Science.gov (United States)

Gonzalo-Lumbreras, Raquel; Sanz-Landaluze, Jon; Cámara, Carmen

2015-07-01

The behavior of 15 benzimidazoles, including their main metabolites, using several C18 columns with standard or narrow-bore diameters and different particle size and type were evaluated. These commercial columns were selected because their differences could affect separation of benzimidazoles, and so they can be used as alternative columns. A simple screening method for the analysis of benzimidazole residues and their main metabolites was developed. First, the separation of benzimidazoles was optimized using a Kinetex C18 column; later, analytical performances of other columns using the above optimized conditions were compared and then individually re-optimized. Critical pairs resolution, analysis run time, column type and characteristics, and selectivity were considered for chromatographic columns comparison. Kinetex XB was selected because it provides the shortest analysis time and the best resolution of critical pairs. Using this column, the separation conditions were re-optimized using a factorial design. Separations obtained with the different columns tested can be applied to the analysis of specific benzimidazoles residues or other applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Studies on improved integrated membrane-based chromatographic process for bioseparation

Science.gov (United States)

Xu, Yanke

To improve protein separation and purification directly from a fermentation broth, a novel membrane filtration-cum-chromatography device configuration having a relatively impermeable coated zone near the hollow fiber module outlet has been developed. The integrated membrane filtration-cum-chromatography unit packed with chromatographic beads on the shell side of the hollow fiber unit enjoys the advantages of both membrane filtration and chromatography; it allows one to load the chromatographic media directly from the fermentation broth or lysate and separate the adsorbed proteins through the subsequent elution step in a cyclic process. Interfacial polymerization was carried out to coat the bottom section of the hollow fiber membrane while leaving the rest of the hollow fiber membrane unaffected. Myoglobin (Mb), bovine serum albumin (BSA) and a-lactalbumin (a-LA) were used as model proteins in binary mixtures. Separation behaviors of binary protein mixtures were studied in devices using either an ultrafiltration (UF) membrane or a microfiltration (MF) membrane. Experimental results show that the breakthrough time and the protein loading capacities were dramatically improved after coating in both UF and MF modules. For a synthetic yeast fermentation broth feed, the Mb and a-LA elution profiles for the four consecutive cyclic runs were almost superimposable. Due to the lower transmembrane flux in this device plus the periodical washing-elution during the chromatographic separation, fouling was not a problem as it is in conventional microfiltration. A mathematical model describing the hydrodynamic and protein loading behaviors of the integrated device using UF membrane with a coated zone was developed. The simulation results for the breakthrough agree well with the experimental breakthrough curves. The optimal length of the coated zone was obtained from the simulation. A theoretical analysis of the protein mass transfer was performed using a diffusion-convection model

In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores

Energy Technology Data Exchange (ETDEWEB)

Cheng Hefa [State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Reinhard, Martin, E-mail: reinhard@stanford.edu [Department of Civil and Environmental Engineering, Stanford University, Stanford, CA 94305-4020 (United States)

2010-07-15

Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microprous solids and investigating contaminant-solid interactions.

In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores

International Nuclear Information System (INIS)

Cheng Hefa; Reinhard, Martin

2010-01-01

Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microprous solids and investigating contaminant-solid interactions.

In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores.

Science.gov (United States)

Cheng, Hefa; Reinhard, Martin

2010-07-15

Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microporous solids and investigating contaminant-solid interactions. 2010 Elsevier B.V. All rights reserved.

Standardization of Berberis aristata extract through conventional and modern HPTLC techniques

Directory of Open Access Journals (Sweden)

Dinesh K. Patel

2012-05-01

Full Text Available Objective: Berberis aristata (Berberidaceae is an important medicinal plant, found in the different region of the world. It has significant medicinal value in the traditional Indian and Chinese system of medicine. The aim of the present investigation includes qualitative and quantitative analysis of Berberis aristata extract. Methods: Present study includes determination of phytochemical analysis, solubility test, heavy metal analysis, antimicrobial study and quantitative analysis by HPTLC method. Results: Preliminary phytochemical analysis showed the presence of carbohydrate, glycoside, alkaloid, protein, amino acid, saponin, tannin and flavonoid. Solubility in water and alcohal were found to be 81.90% in water and 84.52% in 50% in alcohal. Loss on drying was found to be 5.32%. Total phenol and flavonoid content were found to be 0.11% and 2.8%. Level of lead, arsenic, mercury and cadmium complies the standard level. E. coli and salmonella was found to be absent whereas total bacterial count, yeast and moulds contents were found to be under the limit. Content of berberine was found to be 13.47% through HPTLC techniques. Conclusions: The results obtained from the present studies could be used as source of valuable information which can play an important role for the food scientists, researchers and even the consumers for its standards.

A Gas Chromatographic Method for the Determination of Bicarbonate and Dissolved Gases

Directory of Open Access Journals (Sweden)

John H. Loughrin

2017-11-01

Full Text Available A gas chromatographic method for the rapid determination of aqueous carbon dioxide and its speciation into solvated carbon dioxide and bicarbonate is presented. One-half mL samples are injected through a rubber septum into 20-mL vials that are filled with 9.5 mL of 0.1 N HCl. A one mL portion of the headspace is withdrawn and injected onto a gas chromatograph equipped with a thermal conductivity detector. Using the dimensionless Henry's constant for carbon dioxide and an adaptation of the Henderson-Hasselbalch equation, carbon dioxide in the samples can be categorized among solvated, bicarbonate, and carbonate forms. Natural water samples as well as wastewater from a municipal sewage treatment plant and a swine rearing operation were analyzed by this method and the results compared favorably to those obtained by titration. Samples stored for up to 5 weeks showed no significant changes in carbon dioxide concentrations. In addition, using flame ionization and electron capture detectors, methane and nitrous oxide concentrations in the samples were also measured.

Chromatographic Monoliths for High-Throughput Immunoaffinity Isolation of Transferrin from Human Plasma

Directory of Open Access Journals (Sweden)

Irena Trbojević-Akmačić

2016-06-01

Full Text Available Changes in protein glycosylation are related to different diseases and have a potential as diagnostic and prognostic disease biomarkers. Transferrin (Tf glycosylation changes are common marker for congenital disorders of glycosylation. However, biological interindividual variability of Tf N-glycosylation and genes involved in glycosylation regulation are not known. Therefore, high-throughput Tf isolation method and large scale glycosylation studies are needed in order to address these questions. Due to their unique chromatographic properties, the use of chromatographic monoliths enables very fast analysis cycle, thus significantly increasing sample preparation throughput. Here, we are describing characterization of novel immunoaffinity-based monolithic columns in a 96-well plate format for specific high-throughput purification of human Tf from blood plasma. We optimized the isolation and glycan preparation procedure for subsequent ultra performance liquid chromatography (UPLC analysis of Tf N-glycosylation and managed to increase the sensitivity for approximately three times compared to initial experimental conditions, with very good reproducibility. This work is licensed under a Creative Commons Attribution 4.0 International License.

Leveraging probabilistic peak detection to estimate baseline drift in complex chromatographic samples.

Science.gov (United States)

Lopatka, Martin; Barcaru, Andrei; Sjerps, Marjan J; Vivó-Truyols, Gabriel

2016-01-29

Accurate analysis of chromatographic data often requires the removal of baseline drift. A frequently employed strategy strives to determine asymmetric weights in order to fit a baseline model by regression. Unfortunately, chromatograms characterized by a very high peak saturation pose a significant challenge to such algorithms. In addition, a low signal-to-noise ratio (i.e. s/npeak detection algorithm. A posterior probability of being affected by a peak is computed for each point in the chromatogram, leading to a set of weights that allow non-iterative calculation of a baseline estimate. For extremely saturated chromatograms, the peak weighted (PW) method demonstrates notable improvement compared to the other methods examined. However, in chromatograms characterized by low-noise and well-resolved peaks, the asymmetric least squares (ALS) and the more sophisticated Mixture Model (MM) approaches achieve superior results in significantly less time. We evaluate the performance of these three baseline correction methods over a range of chromatographic conditions to demonstrate the cases in which each method is most appropriate. Copyright © 2016 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic method for guanylhydrazone compounds.

Science.gov (United States)

Cerami, C; Zhang, X; Ulrich, P; Bianchi, M; Tracey, K J; Berger, B J

1996-01-12

A high-performance liquid chromatographic method has been developed for a series of aromatic guanylhydrazones that have demonstrated therapeutic potential as anti-inflammatory agents. The compounds were separated using octadecyl or diisopropyloctyl reversed-phase columns, with an acetonitrile gradient in water containing heptane sulfonate, tetramethylammonium chloride, and phosphoric acid. The method was used to reliably quantify levels of analyte as low as 785 ng/ml, and the detector response was linear to at least 50 micrograms/ml using a 100 microliters injection volume. The assay system was used to determine the basic pharmacokinetics of a lead compound, CNI-1493, from serum concentrations following a single intravenous injection in rats.

Occurrence of curcuminoids in Curcuma longa : A quality standardization by HPTLC

Directory of Open Access Journals (Sweden)

M Paramasivam

2008-06-01

Full Text Available A simple high performance thin layer chromatographic (HPTLC method has been developed for the simultaneous determination of the pharmacologically important active Curcuminoids viz. curcumin, demthoxycurcumin and bis-demethoxycurcumin in Curcuma longa L. The assay combines the separation and quantification of the analytes on silica gel 60 GF254 HPTLC plates with visualisation under UV and scanning at 425 nm. Using this technique, the alkaloidal content of different parts of the title plant has been determined.

Element selective detection of molecular species applying chromatographic techniques and diode laser atomic absorption spectrometry.

Science.gov (United States)

Kunze, K; Zybin, A; Koch, J; Franzke, J; Miclea, M; Niemax, K

2004-12-01

Tunable diode laser atomic absorption spectroscopy (DLAAS) combined with separation techniques and atomization in plasmas and flames is presented as a powerful method for analysis of molecular species. The analytical figures of merit of the technique are demonstrated by the measurement of Cr(VI) and Mn compounds, as well as molecular species including halogen atoms, hydrogen, carbon and sulfur.

Gas chromatographic studies of the relative retention of the sulfur isotopes in carbonyl sulfide, carbon disulfide, and sulfur dioxide

International Nuclear Information System (INIS)

Fetzer, J.C.; Rogers, L.B.

1980-01-01

A precision gas chromatograph, coupled to a quadrupole mass spectrometer and an on-line computer, was used to study the fractionation on Porasil A of the 32 S/ 34 S isotopic pair in a variety of sulfur-containing molecules. Carbonyl sulfide (COS) yielded an average α value of 1.00074 +- 0.00017 (standard deviation) for the temperature range 25 0 C to 75 0 C. The carbon disulfide (CS 2 ) value was 1.00069 +- 0.00023 for the range 53 0 C to 103 0 C, and that for sulfur dioxide (SO 2 ) was 1.00090 +- 0.00018 for the range 62 0 C to 112 0 C. Differential thermodynamic data have been reported. A Porapak Q column showed no fractionation of this isotopic pair in these three molecules

Second-order Data by Flow Injection Analysis with Spectrophotometric Diode-array Detection and Incorporated Gel-filtration Chromatographic Column

DEFF Research Database (Denmark)

Bechmann, Iben Ellegaard

1997-01-01

A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate(III) and he......A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate...

OpenChrom: a cross-platform open source software for the mass spectrometric analysis of chromatographic data.

Science.gov (United States)

Wenig, Philip; Odermatt, Juergen

2010-07-30

Today, data evaluation has become a bottleneck in chromatographic science. Analytical instruments equipped with automated samplers yield large amounts of measurement data, which needs to be verified and analyzed. Since nearly every GC/MS instrument vendor offers its own data format and software tools, the consequences are problems with data exchange and a lack of comparability between the analytical results. To challenge this situation a number of either commercial or non-profit software applications have been developed. These applications provide functionalities to import and analyze several data formats but have shortcomings in terms of the transparency of the implemented analytical algorithms and/or are restricted to a specific computer platform. This work describes a native approach to handle chromatographic data files. The approach can be extended in its functionality such as facilities to detect baselines, to detect, integrate and identify peaks and to compare mass spectra, as well as the ability to internationalize the application. Additionally, filters can be applied on the chromatographic data to enhance its quality, for example to remove background and noise. Extended operations like do, undo and redo are supported. OpenChrom is a software application to edit and analyze mass spectrometric chromatographic data. It is extensible in many different ways, depending on the demands of the users or the analytical procedures and algorithms. It offers a customizable graphical user interface. The software is independent of the operating system, due to the fact that the Rich Client Platform is written in Java. OpenChrom is released under the Eclipse Public License 1.0 (EPL). There are no license constraints regarding extensions. They can be published using open source as well as proprietary licenses. OpenChrom is available free of charge at http://www.openchrom.net.

Determination of trihalomethanes in waters by ionic liquid-based single drop microextraction/gas chromatographic/mass spectrometry.

Science.gov (United States)

Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

2008-10-31

A simple, rapid, solventless method for the determination of trihalomethanes (THMs) (chloroform, bromodichloromethane, dibromochloromethane and bromoform) in water samples is presented. The analytes are extracted from the headspace of the aqueous matrix into a 2 microL drop of the ionic liquid 1-octyl-3-methyl-imidazolium hexafluorophosphate working at 30 degrees C for 30 min. The separation and detection of the target compounds is accomplished by gas chromatography/mass spectrometry owing to the use of an interface that efficiently transfers the analytes extracted in the ionic liquid drop to the gas chromatograph while preventing the ionic liquid from entering the column. The detection limits obtained are below the values compelled by the legislation, ranging from 0.5 microg L(-1) for chloroform and bromodichloromethane to 0.9 microg L(-1) for dibromochloromethane. The use of ionic liquid in the extraction procedure avoids the use of organic solvents and leads to relative standard deviations that range from 3.1% to 4.8%.

High-performance liquid chromatographic assay for two rifamycin-derived hypocholesterolemic agents in liver and biological fluids.

Science.gov (United States)

Moore, D J; Perrino, P J; Klerer, C P; Robertson, P

1993-02-26

CGP 43371 (compound I), a mono-pivaloyl oxazole derivative of a 3-piperazino-rifamycin, has been in clinical trials as a potential hypocholesterolemic agent. A reversed-phase high-performance liquid chromatographic (HPLC) assay was developed using a C18 column and a gradient solvent system of methanol-0.1 M sodium acetate, pH 4.5, at a flow-rate of 1 ml/min. The compound and internal standard (rifampicin) were detected by their ultraviolet absorption at 254 nm. Isolation of the compounds from plasma and liver homogenates was accomplished by precipitation of proteins with acetonitrile, followed by evaporation under nitrogen and reconstitution in methanol. Bile, lymph and urine were injected onto the HPLC column without pretreatment. Calibration curves were linear (r > 0.999) over the concentration range 0.25-20.0 micrograms/ml. The assay procedure was also applicable to other rifamycin derivatives and was able to distinguish between molecular species containing small differences in functionality.

Chromatographic methods for the simultaneous determination of binary mixture of Saxagliptin HCl and Metformin HCl

Directory of Open Access Journals (Sweden)

Hanan A. Merey

2017-12-01

Full Text Available Two chromatographic methods were suggested for the simultaneous determination of a binary mixture containing Saxagliptin HCl (SAG and Metformin HCl (MET. First method was RP-HPLC method. Chromatographic separation was done on Kinetex™ column–C18 (4.6 × 150 mm, 2.6 µm using mobile phase consisted of acetonitrile:phosphate buffer pH = 4.5 ± 0.1 adjusted with orthophosphoric acid (13:87, v/v. Isocratic elution at a flow rate 1.5 mL/min and UV detection at 220.0 nm was performed. Second method was spectro-densitometric method. Chromatographic separation was done on precoated silica gel aluminium plates 60 F254 as a stationary phase and developing system consisting of chloroform:methanol:formic acid (80:20:0.3, by volume. The density of the separated bands was measured by UV detector at 210.0 nm. The proposed methods were validated as per the ICH guidelines parameters like Linearity, precision, accuracy, selectivity, limit of detection and limit of quantitation. Statistical comparison was done between the obtained results and those obtained by the reported methods, showing no significant difference with respect to accuracy and precision. Keywords: Saxagliptin HCl, Metformin HCl, RP-HPLC, TLC

Open Partial Nephrectomy in Renal Cancer: A Feasible Gold Standard Technique in All Hospitals

Directory of Open Access Journals (Sweden)

J. M. Cozar

2008-01-01

Full Text Available Introduction. Partial nephrectomy (PN is playing an increasingly important role in localized renal cell carcinoma (RCC as a true alternative to radical nephrectomy. With the greater experience and expertise of surgical teams, it has become an alternative to radical nephrectomy in young patients when the tumor diameter is 4 cm or less in almost all hospitals since cancer-specific survival outcomes are similar to those obtained with radical nephrectomy. Materials and Methods. The authors comment on their own experience and review the literature, reporting current indications and outcomes including complications. The surgical technique of open partial nephrectomy is outlined. Conclusions. Nowadays, open PN is the gold standard technique to treat small renal masses, and all nonablative techniques must pass the test of time to be compared to PN. It is not ethical for patients to undergo radical surgery just because the urologists involved do not have adequate experience with PN. Patients should be involved in the final treatment decision and, when appropriate, referred to specialized centers with experience in open or laparoscopic partial nephrectomies.

Chromatographic analyses of fatty acid methyl esters by HPLC-UV and GC-FID

Energy Technology Data Exchange (ETDEWEB)

Carvalho, Myller S.; Pinho, David M.M.; Suarez, Paulo A.Z., E-mail: psuarez@unb.br [Laboratorio de Materiais e Combustiveis, Instituto de Quimica, Universidade de Brasilia, DF (Brazil); Mendonca, Marcio A. [Faculdade de Agronomia e Medicina Veterinaria, Universidade de Brasilia, DF (Brazil); Resck, Ines S. [Laboratorio de Ressonancia Magnetica Nuclear, Universidade de Brasilia, DF (Brazil)

2012-04-15

An analytical method using high performance liquid chromatography with UV detection (HPLC-UV) (method A) was used for simultaneous determination of total amounts of triacylglycerides, diacylglycerides, monoacylglycerides and fatty acid methyl esters in alcoholysis of different oil (cotton, canola, sunflower, corn and soybean) samples. Analyses were carried out at 40 deg C for 20 min using a gradient of methanol (MeOH) and 2-propanol-hexane 5:4 (v/v) (PrHex): 100% of MeOH in 0 min, 50% of MeOH and 50% of PrHex in 10 min maintained with isocratic elution for 10 min. Another HPLC-UV method (method B) with acetonitrile isocratic elution for 34 min was used to determine the fatty acid composition of oils analyzing their methyl ester derivatives. Contents were determined with satisfactory repeatability (relative standard deviation, RSD < 3%), linearity (r{sup 2} > 0.99) and sensitivity (limit of quantification). Method B was compared with an official gas chromatographic method with flame ionization detection (GC-FID) from American Oil Chemists' Society (AOCS) in the determination of fatty acid methyl esters (FAME) in biodiesel real samples. (author)

Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

Energy Technology Data Exchange (ETDEWEB)

Liu, Ying [Iowa State Univ., Ames, IA (United States)

2004-01-01

My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

International Nuclear Information System (INIS)

Ying Liu

2004-01-01

My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

Measurement Uncertainty of Liquid Chromatographic Analyses Visualized by Ishikawa Diagrams

OpenAIRE

Meyer, Veronika R.

2017-01-01

Ishikawa, or cause-and-effect diagrams, help to visualize the parameters that influence a chromatographic analysis. Therefore, they facilitate the set up of the uncertainty budget of the analysis, which can then be expressed in mathematical form. If the uncertainty is calculated as the Gaussian sum of all uncertainty parameters, it is necessary to quantitate them all, a task that is usually not practical. The other possible approach is to use the intermediate precision as a base for the uncer...

Chromatographic separation of europium and gadolinum mixtures by ethylenediaminedisuccinic acid

International Nuclear Information System (INIS)

Kolleganov, M.Yu.; Nazarov, P.P.; Martynenko, L.I.; Mtrofanova, N.D.; Spitsyn, V.I.

1985-01-01

Comparative investigation of chromatographic separation of impurities of Eu and Gd micro- and macroquantities by means of ethylenediaminedisuccinic (EDDS) and ethylene-diaminetetraacetic (EDTA) acids is performed. It is shown that EDTA is a sufficiently effective agent for separation of this pair of elements. The values of EU and Gd separation coefficients obtained in experiments with RE microquantities are not realized at Eu-Gd, macroquantities separation which probably is connected with the influence of polymerization processes in the systems containing RE and EDDS complexes

New extraction chromatographic material for rhenium separation

International Nuclear Information System (INIS)

Lucanikova, M.; Czech Technical University, Prague; Kucera, J.; Czech Technical University, Prague; Sebesta, F.

2008-01-01

Three types of the extraction chromatographic materials, composed from Aliquat R 336 deposited in the polyacrylonitrile (PAN) beads and prepared by different procedures, were compared for extraction of rhenium. The best properties were exhibited when the solid extractant was prepared by impregnation of the ready-made PAN beads. Solid extractant prepared by direct coagulation of the beads from the suspension of Aliquat R 336 in solution of PAN in nitric acid differs only by lower capacity in dynamic conditions. Material prepared from the PAN solution in dimethylsulfoxide was the worst because Aliquat R 336 was washed out from the beads during coagulation of the polymer and the extraction capacity was low. As it is shown, the first two solid extractants are fully comparable with the commercial TEVA Resin. (author)

Suspect screening of large numbers of emerging contaminants in environmental waters using artificial neural networks for chromatographic retention time prediction and high resolution mass spectrometry data analysis.

Science.gov (United States)

Bade, Richard; Bijlsma, Lubertus; Miller, Thomas H; Barron, Leon P; Sancho, Juan Vicente; Hernández, Felix

2015-12-15

The recent development of broad-scope high resolution mass spectrometry (HRMS) screening methods has resulted in a much improved capability for new compound identification in environmental samples. However, positive identifications at the ng/L concentration level rely on analytical reference standards for chromatographic retention time (tR) and mass spectral comparisons. Chromatographic tR prediction can play a role in increasing confidence in suspect screening efforts for new compounds in the environment, especially when standards are not available, but reliable methods are lacking. The current work focuses on the development of artificial neural networks (ANNs) for tR prediction in gradient reversed-phase liquid chromatography and applied along with HRMS data to suspect screening of wastewater and environmental surface water samples. Based on a compound tR dataset of >500 compounds, an optimized 4-layer back-propagation multi-layer perceptron model enabled predictions for 85% of all compounds to within 2min of their measured tR for training (n=344) and verification (n=100) datasets. To evaluate the ANN ability for generalization to new data, the model was further tested using 100 randomly selected compounds and revealed 95% prediction accuracy within the 2-minute elution interval. Given the increasing concern on the presence of drug metabolites and other transformation products (TPs) in the aquatic environment, the model was applied along with HRMS data for preliminary identification of pharmaceutically-related compounds in real samples. Examples of compounds where reference standards were subsequently acquired and later confirmed are also presented. To our knowledge, this work presents for the first time, the successful application of an accurate retention time predictor and HRMS data-mining using the largest number of compounds to preliminarily identify new or emerging contaminants in wastewater and surface waters. Copyright © 2015 Elsevier B.V. All rights

Chromatographic profiles of extractives from leaves of Eugenia uniflora

Directory of Open Access Journals (Sweden)

Isabelle C.F. Bezerra

Full Text Available ABSTRACT Eugenia uniflora L., Myrtaceae, popularly known as “pitanga”, is used in traditional medicine due the properties attributed to its chemical content, these being mainly hydrolysable tannins and flavonoids. This study provides a qualitative and quantitative evaluation of chemical profile from leaves of E. uniflora. The HPLC analysis was carried out on a C18 column (4.6 mm × 250 mm, 5 µm by gradient elution with methanol and water (acidified with trifluoracetic acid; and silica gel Plates 60-F 254 with 10–12 µm and 5–6 µm particles, respectively for TLC and High HPTLC analysis. The chromatographic data obtained from HPLC, TLC and HPTLC presented bands and peaks related to flavonoids (myricitrin and derivatives and tannins (gallic and ellagic acids, which were observed from different samples. The chromatographic similarities enabled the building of a typical fingerprint for the herbal material. The similarity analysis of the sample data by Pearson correlation showed R values >0.9 among peaks (HPLC and bands (HPTLC. In addition, the analytical methodology developed by HPLC enabled the satisfactory quantification of marker substances [ellagic acid = 0.22% and 0.20% (m/m; gallic acid = 0.20% and 0.43%; myricitrin = 0.42 and 1.74% (m/m in herbal drug and crude extract, respectively]. The procedure was also validated in accordance with the assays required by Brazilian legislation. Thus, the HPTLC and HPLC methods developed in this study provide helpful and simple tools for the quality evaluation both qualitatively and quantitatively of raw materials and extractives from leaves of E. uniflora.

Study PWA8 resin for chromatographic uranium concentration

International Nuclear Information System (INIS)

Coceancigh, Herman; Ramella, J. L.; Marrero, Julieta; Jiménez Rebagliati, Raúl

2013-01-01

For many years nuclear industry have been using resins as filler of chromatographic columns. These methods are specific and give reliable results in different applications, for those reasons are extremely useful as separation process. Currently the nuclear industry is growing and this brings new issues such as the need of reduction of the amount of waste, the optimization of the production process and others that the chromatography could solve with great results. AMBERLITETM PWA8 resin is an anion exchange resin which can be used for the removal of uranium from drinking water. In addition to high exchange capacity, this resin has excellent physical stability and a wide range of pH in which is operational. With the idea of concentrating uranium from wastes solution as main goal we made different experiments to understand the AMBERLITETM PWA8 and obtain the most important characteristics like; pH working range; capacity; activation and elution procedures. These procedures were developed and optimized the capacity was determined using a batch experiment and we obtain that the maximum capacity is 882,5 U ug /resin gr at a pH of 4,2. Following on from these results chromatographic experiments were performed in which both were obtained the percentage of recovery and the concentration factor. The percent recovery (% R) calculated as the percentage ratio between the total mass and the load mass eluted (% R = eluted mass / total mass * 100) was 94% with a concentration factor of 5 times From these results it is intended to concentrate wastes solutions from the fuel cycle processes with two main goals: decreasing volume for storage and for future reusing of the uranium coming from production. (author)

Subsurface migration of petroleum hydrocarbons: A case study of immiscible migration and chromatographic separation

International Nuclear Information System (INIS)

Dawson, H.E.

1991-01-01

The subsurface distribution of a leaked crude oil illustrates the combined influence of both the chemical and physical properties of soil and free product on the migration of petroleum hydrocarbons. Immiscible phase behavior was observed, as well as chromatographic-like separation of the lighter constituents of the crude oil from the heavier constituents. After downward migration through approximately 50 ft of unsaturated, heterogeneous alluvial sediments, the crude oil formed a horizontal plume on top of a perched, saturated zone. Immiscible phase trapping is evident from the occurrence of very high concentration of hydrocarbons in both the vertical and horizontal plumes. Samples taken from the vertical zone of contamination indicate a transition from heavier hydrocarbons near the surface to lighter hydrocarbons at depth. This phenomenon is attributed to chromatographic-like separation of the heavier hydrocarbons by the soil, possibly due to preferential solubility of the lighter hydrocarbons in percolating ran water

ANALYSIS OF DISSOLVED METHANE, ETHANE, AND ETHYLENE IN GROUND WATER BY A STANDARD GAS CHROMATOGRAPHIC TECHNIQUE

Science.gov (United States)

The measurement of dissolved gases such as methane, ethane, and ethylene in ground water is important in determining whether intrinsic bioremediation is occurring in a fuel- or solvent-contaminated aquifer. A simple procedure is described for the collection and subsequent analys...

Procedure for the production of PZC based chromatographic Tc-99m generator to be available for clinical application

International Nuclear Information System (INIS)

Le Van So; Pham Ngoc Dien; Truong Hong Nghia; Nguyen Thi Thu; Nguyen Cong Duc; Vo Thi Cam Hoa; Bui Van Cuong

2004-01-01

The chemical synthesis for the preparation of polymer compound of Zirconium (PZC) and the column pre-loading procedure for the preparation of PZC based chromatographic Tc-99m generators were described in detail. In-process documentation, flow-chart of process, specific Tc-99m generator designs and picturially illustrative description of Tc-99 generator production process were systematically reported. The column pre-loading procedure was highly evaluated as a competent technology for the preparation of PZC based Tc-99m chromatographic generator of high performance using (n,γ) 99 Mo of low specific radioactivity produced on low power research reactors. (author)

Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

Directory of Open Access Journals (Sweden)

Serpil Sevim

2015-12-01

Full Text Available abstract The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4 and acetonitrile (35:65 by volume. The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL and limit of quantification (50 ng/mL were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000. In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method.

Study of stationary phase stability from a column with chromatographic material for steady state treatment of an effluent and/or waste containing Th-232

International Nuclear Information System (INIS)

Felinto, Maria Claudia Franca da Cunha; Martinz, Daniel Ortiz

1999-01-01

This work relates the behavior of a new chromatographic material, AMBERCMPO I, that has been studied to remove actinide elements from the High Level Liquid Waste. It gives emphasis to the behavior of chromatographic materials to the extraction of Th 4+ and its performance after some operation cycle. (author)

Improving accuracy and precision of ice core δD(CH4 analyses using methane pre-pyrolysis and hydrogen post-pyrolysis trapping and subsequent chromatographic separation

Directory of Open Access Journals (Sweden)

M. Bock

2014-07-01

Full Text Available Firn and polar ice cores offer the only direct palaeoatmospheric archive. Analyses of past greenhouse gas concentrations and their isotopic compositions in air bubbles in the ice can help to constrain changes in global biogeochemical cycles in the past. For the analysis of the hydrogen isotopic composition of methane (δD(CH4 or δ2H(CH4 0.5 to 1.5 kg of ice was hitherto used. Here we present a method to improve precision and reduce the sample amount for δD(CH4 measurements in (ice core air. Pre-concentrated methane is focused in front of a high temperature oven (pre-pyrolysis trapping, and molecular hydrogen formed by pyrolysis is trapped afterwards (post-pyrolysis trapping, both on a carbon-PLOT capillary at −196 °C. Argon, oxygen, nitrogen, carbon monoxide, unpyrolysed methane and krypton are trapped together with H2 and must be separated using a second short, cooled chromatographic column to ensure accurate results. Pre- and post-pyrolysis trapping largely removes the isotopic fractionation induced during chromatographic separation and results in a narrow peak in the mass spectrometer. Air standards can be measured with a precision better than 1‰. For polar ice samples from glacial periods, we estimate a precision of 2.3‰ for 350 g of ice (or roughly 30 mL – at standard temperature and pressure (STP – of air with 350 ppb of methane. This corresponds to recent tropospheric air samples (about 1900 ppb CH4 of about 6 mL (STP or about 500 pmol of pure CH4.

Environmental Technology Verification Report. Field Portable Gas Chromatograph/Mass Spectrometer. Viking Instruments Corporation SpectraTrak (Trademark) 672

National Research Council Canada - National Science Library

Enfield, Wayne

1997-01-01

.... This self-contained, field transportable system, whose design has been adapted from laboratory technology, uses a contained, chromatographic column and accompanying mass spectrometer to provide...

Efficient fabrication of high-capacity immobilized metal ion affinity chromatographic media: The role of the dextran-grafting process and its manipulation.

Science.gov (United States)

Zhao, Lan; Zhang, Jingfei; Huang, Yongdong; Li, Qiang; Zhang, Rongyue; Zhu, Kai; Suo, Jia; Su, Zhiguo; Zhang, Zhigang; Ma, Guanghui

2016-03-01

Novel high-capacity Ni(2+) immobilized metal ion affinity chromatographic media were prepared through the dextran-grafting process. Dextran was grafted to an allyl-activated agarose-based matrix followed by functionalization for the immobilized metal ion affinity chromatographic media. With elaborate regulation of the allylation degree, dextran was completely or partly grafted to agarose microspheres, namely, completely dextran-grafted agarose microspheres and partly dextran-grafted ones, respectively. Confocal laser scanning microscope results demonstrated that a good adjustment of dextran-grafting degree was achieved, and dextran was distributed uniformly in whole completely dextran-grafted microspheres, while just distributed around the outside of the partly dextran-grafted ones. Flow hydrodynamic properties were improved greatly after the dextran-grafting process, and the flow velocity increased by about 30% compared with that of a commercial chromatographic medium (Ni Sepharose FF). A significant improvement of protein binding performance was also achieved by the dextran-grafting process, and partly dextran-grafted Ni(2+) chelating medium had a maximum binding capacity for His-tagged lactate dehydrogenase about 2.5 times higher than that of Ni Sepharose FF. The results indicated that this novel chromatographic medium is promising for applications in high-efficiency and large-scale protein purification. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Estimations of temperature deviations in chromatographic columns using isenthalpic plots. I. Theory for isocratic systems.

Science.gov (United States)

Tarafder, Abhijit; Iraneta, Pamela; Guiochon, Georges; Kaczmarski, Krzysztof; Poe, Donald P

2014-10-31

We propose to use constant enthalpy or isenthalpic diagrams as a tool to estimate the extent of the temperature variations caused by the mobile phase pressure drop along a chromatographic column, e.g. of its cooling in supercritical fluid and its heating in ultra-performance liquid chromatography. Temperature strongly affects chromatographic phenomena. Any of its variations inside the column, whether intended or not, can lead to significant changes in separation performance. Although instruments use column ovens in order to keep constant the column temperature, operating conditions leading to a high pressure drop may cause significant variations of the column temperature, both in the axial and the radial directions, from the set value. Different ways of measuring these temperature variations are available but they are too inconvenient to be employed in many practical situations. In contrast, the thermodynamic plot-based method that we describe here can easily be used with only a ruler and a pencil. They should be helpful in developing methods or in analyzing results in analytical laboratories. Although the most effective application area for this approach should be SFC (supercritical fluid chromatography), it can be applied to any chromatographic conditions in which temperature variations take place along the column due to the pressure drop, e.g. in ultra-high pressure liquid chromatography (UHPLC). The method proposed here is applicable to isocractic conditions only. Copyright © 2014 Elsevier B.V. All rights reserved.

Advanced Packaging Materials and Techniques for High Power TR Module: Standard Flight vs. Advanced Packaging

Science.gov (United States)

Hoffman, James Patrick; Del Castillo, Linda; Miller, Jennifer; Jenabi, Masud; Hunter, Donald; Birur, Gajanana

2011-01-01

The higher output power densities required of modern radar architectures, such as the proposed DESDynI [Deformation, Ecosystem Structure, and Dynamics of Ice] SAR [Synthetic Aperture Radar] Instrument (or DSI) require increasingly dense high power electronics. To enable these higher power densities, while maintaining or even improving hardware reliability, requires advances in integrating advanced thermal packaging technologies into radar transmit/receive (TR) modules. New materials and techniques have been studied and compared to standard technologies.

Gas-chromatographic quantitative determination of argon in air samples, by elimination of oxigen

International Nuclear Information System (INIS)

Sofronie, E.

1982-08-01

A method of gas-chromatographic quantitative determination of argon in air samples, by elimination of oxygen, is presented. Experiments were carried out in a static system. Conditions for the application of the method in dynamic systems are specified. Sensibility of the method: 5 10 -4 cm 3 Ar per cm 3 of air. (author)

The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

Energy Technology Data Exchange (ETDEWEB)

Soran, Maria Loredana; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Cobzac, Simona Codruta, E-mail: loredana.soran@itim-cj.r [Babes-Bolyai University, Faculty of Chemistry and Chemical Engineering, 11 Arany Janos, 400028 Cluj-Napoca (Romania)

2009-08-01

Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: {alpha} and {beta}-pinene (mixture), limonene, citronellol, and geraniol.

The extraction and chromatographic determination of the essentials oils from Ocimum basilicum L. by different techniques

International Nuclear Information System (INIS)

Soran, Maria Loredana; Varodi, Codruta; Lung, Ildiko; Surducan, Emanoil; Surducan, Vasile; Cobzac, Simona Codruta

2009-01-01

Three different techniques (maceration, sonication and extraction in microwave field) were used for extraction of essential oils from Ocimum basilicum L. The extracts were analyzed by TLC/HPTLC technique and the fingerprint informations were obtained. The GC-FID was used to characterized the extraction efficiency and for identify the terpenic bioactive compounds. The most efficient extraction technique was maceration followed by microwave and ultrasound. The best extraction solvent system was ethyl ether + ethanol (1:1, v/v). The main compounds identified in Ocimum basilicum L. extracts were: α and β-pinene (mixture), limonene, citronellol, and geraniol.

High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

Science.gov (United States)

A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

[Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up].

Science.gov (United States)

Zhang, Chunyu; Wang, Hui; Zhang, Xiaohui; Ma, Zhongqiang; Deng, Wanmei; Hu, Ke; Ding, Mingyu

2011-12-01

A method of gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) was established for the simultaneous determination of 5 main phthalate plasticizers in foods (edible oil, instant noodles, fried pastries, Saqima, etc.). The samples were extracted with petroleum ether in an ultrasonator, purified by a GPC column, and analyzed by HPLC. The chromatographic separation was achieved on a Labtech-C18 column (250 mm x 4.6 mm, 5 microm) using acetonitrile and water mixture as the mobile phases in a gradient elution mode. The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25 - 13.4 microg/L. The spike recoveries were between 70.4% and 113.6% with the relative standard deviations (RSDs, n = 3) of 0.3% - 5.8% at the spiked level of 50 mg/L. This method is simple, rapid and practical, and can be used for the simultaneous determination of PAEs in grease food samples.

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

Science.gov (United States)

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

2017-04-15

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

Aligning of single and multiple wavelength chromatographic

DEFF Research Database (Denmark)

Nielsen, Niels-Peter Vest; Carstensen, Jens Michael; Smedsgaard, Jørn

1998-01-01

optimised warping (COW) using two input parameters which can be estimated from the observed peak width. COW is demonstrated on constructed single trace chromatograms and on single and multiple wavelength chromatograms obtained from HPLC diode detection analyses of fungal extractsA copy of the C program......The use of chemometric data processing is becoming an important part of modern chromatography. Most chemometric analyses are performed on reduced data sets using areas of selected peaks detected in the chromatograms, which means a loss of data and introduces the problem of extracting peak data from...... to utilise the entire data matrix or rely on peak detection, thus having the same limitations as the commonly used chemometric procedures. The method presented uses the entire chromatographic data matrices and does not require any preprocessing e.g., peak detection. It relies on piecewise linear correlation...

Authentication and distinction of Shenmai injection with HPLC fingerprint analysis assisted by pattern recognition techniques

Directory of Open Access Journals (Sweden)

Xue-Feng Lu

2012-10-01

Full Text Available In this paper, the feasibility and advantages of employing high performance liquid chromatographic (HPLC fingerprints combined with pattern recognition techniques for quality control of Shenmai injection were investigated and demonstrated. The Similarity Evaluation System was employed to evaluate the similarities of samples of Shenmai injection, and the HPLC generated chromatographic data were analyzed using hierarchical clustering analysis (HCA and soft independent modeling of class analogy (SIMCA. Consistent results were obtained to show that the authentic samples and the blended samples were successfully classified by SIMCA, which could be applied to accurate discrimination and quality control of Shenmai injection. Furthermore, samples could also be grouped in accordance with manufacturers. Our results revealed that the developed method has potential perspective for the original discrimination and quality control of Shenmai injection. Keywords: Shenmai injection, High performance liquid chromatography, Fingerprint, Pattern recognition

Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

Science.gov (United States)

Sun, Jianghao; Chen, Pei

2012-03-05

A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims. Copyright © 2011. Published by Elsevier B.V.

Chromatographic Determination of Toluene and its Metabolites in Urine for Toluene Exposure - A Review

International Nuclear Information System (INIS)

Mohamad Raizul Zinalibdin; Abdul Rahim Yacob; Mohd Marsin Sanagi

2016-01-01

The determinations of toluene and their metabolites in biological samples such as urine and blood allow the estimation of the degree of exposure to this chemical. Chromatographic methods and preliminary methods are now universally employed for this purpose. Preliminary color test methods are well established for qualitative determination of toluene and its metabolites. Mobile test kits using color test methods are a vast tool for screening urine samples but chromatographic methods are still needed for confirmation and quantitative analysis. Gas chromatography (GC) methods are well-adapted for the determination of toluene metabolite in urine, but these methods often require several pretreatment steps. Meanwhile, high performance liquid chromatography (HPLC) is becoming a powerful tool for the accurate and easy determination of toluene metabolites considering its decisive advantages for routine monitoring. Furthermore, recent development in HPLC could widen the usefulness of this method to solve the most complex analytical problems that could be encountered during the measurement. (author)

IMAGING OF FLUOROPHORES IN CHROMATOGRAPHIC BEADS, RECONSTRUCTION OF RADIAL DENSITY DISTRIBUTIONS AND CHARACTERISATION OF PROTEIN UPTAKING PROCESSES

Directory of Open Access Journals (Sweden)

Bernd Stanislawski

2010-11-01

Full Text Available A new adjustment calculus is presented to determine the true intraparticle distribution of bound protein within chromatographic beads from confocal fluorescence slice series. The calculus does not require knowledge about optical properties of different chromatographic materials like refractive index and turbidity, but it depends on a parameter which can be adjusted interactively. The algorithm is of complexity O(n where n is the pixel number. From the reconstructed data we compute the parameters of the protein uptaking process using a model-based approach. It is demonstrated that the protein uptaking rates of the beads strongly dependent on the conditions of the fluid phase influencing the strength of protein surface interaction.

Portable optical frequency standard based on sealed gas-filled hollow-core fiber using a novel encapsulation technique

DEFF Research Database (Denmark)

Triches, Marco; Brusch, Anders; Hald, Jan

2015-01-01

A portable stand-alone optical frequency standard based on a gas-filled hollow-core photonic crystal fiber is developed to stabilize a fiber laser to the 13C2H2 P(16) (ν1 + ν3) transition at 1542 nm using saturated absorption. A novel encapsulation technique is developed to permanently seal...

Adsorption chromatographic separation of radioiodine-labelled compounds using binary eluents

International Nuclear Information System (INIS)

Toth, G.

1980-01-01

An adsorption chromatographic method using Sephadex LH-20 dextran gel as adsorbent and water-organic solvent binary eluents was developed for the systematic separation of low molecular weight radioiodine-labelled substances like iodothyronines, iodobenzoic acids and iodotyrosine methyl ester derivatives of prostaglandins, steroids etc. The adsorbed iodine compounds were separated by water-organic solvent mixture, and the order of the compounds is in accordance with the increasing number of iodine substituents per molecule. A method is reported which enables the calculation of the eluent strength of the water-organic solvent eluents. (author)

Gas chromatographic method fr determination of carbon in metallic uranium

International Nuclear Information System (INIS)

Nikol'skij, V.A.; Markov, V.K.; Evseeva, T.I.; Cherstvenkova, E.P.

1983-01-01

Gas chromatographic device to determine carbon in metal uranium is developed. Burnout unite, permitting to load in the burnout tube simultaneously quite a few (up to 20) weight amounts of materials to be burned is a characteristic feature of the device. As a result amendments for control experiment and determination limit are decreased. The time of a single determination is also reduced. Conditions of carbon burn out from metal uranium are studied and temperature and time of complete extraction of carbon in the form of dioxide from weight amount into gaseous phase are established

Decomposition of pilocarpine eye drops assessed by a highly efficient high pressure liquid chromatographic method

NARCIS (Netherlands)

Kuks, P. F.; Weekers, L. E.; Goldhoorn, P. B.

1990-01-01

A rapid high-resolution high pressure liquid chromatographic method was developed for assaying pilocarpine. Pilocarpine in ophthalmic solutions decomposes fairly rapidly to give isopilocarpine, pilocarpic acid and isopilocarpic acid. The quality of an ophthalmic solution can be assessed by assaying

Correlation of supercritical-fluid extraction recoveries with supercritical-fluid chromatographic retention data: A fundamental study

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

1995-01-01

The possibility of using supercritical-fluid chromatographic retention data for examining the effects of operational parameters, such as pressure and flow rate, on the extraction characteristics in supercritical-fluid extraction (SFE) was investigated. A model was derived for calculating the

Hydrocarbon Fuel Thermal Performance Modeling based on Systematic Measurement and Comprehensive Chromatographic Analysis

Science.gov (United States)

2016-07-31

distribution unlimited Hydrocarbon Fuel Thermal Performance Modeling based on Systematic Measurement and Comprehensive Chromatographic Analysis Matthew...vital importance for hydrocarbon -fueled propulsion systems: fuel thermal performance as indicated by physical and chemical effects of cooling passage... analysis . The selection and acquisition of a set of chemically diverse fuels is pivotal for a successful outcome since test method validation and

Core-shell in liquid chromatography: application for determining sulphonamides in feed and meat using conventional chromatographic systems

Directory of Open Access Journals (Sweden)

Antonio Armentano

2016-12-01

Full Text Available A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-μm column have been optimized on a column packed with 2.6 μm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 μL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster.

Full second order chromatographic/spectrometric data matrices for automated sample identification and component analysis by non-data-reducing image analysis

DEFF Research Database (Denmark)

Nielsen, Niles-Peter Vest; Smedsgaard, Jørn; Frisvad, Jens Christian

1999-01-01

A data analysis method is proposed for identification and for confirmation of classification schemes, based on single- or multiple-wavelength chromatographic profiles. The proposed method works directly on the chromatographic data without data reduction procedures such as peak area or retention...... classes from the reference chromatograms, This feature is a valuable aid in selecting components for further analysis, The identification method is demonstrated on two data sets: 212 isolates from 41 food-borne Penicillium species and 61 isolates from 6 soil-borne Penicillium species. Both data sets...

A New Paradigm for Tissue Diagnostics: Tools and Techniques to Standardize Tissue Collection, Transport, and Fixation.

Science.gov (United States)

Bauer, Daniel R; Otter, Michael; Chafin, David R

2018-01-01

Studying and developing preanalytical tools and technologies for the purpose of obtaining high-quality samples for histological assays is a growing field. Currently, there does not exist a standard practice for collecting, fixing, and monitoring these precious samples. There has been some advancement in standardizing collection for the highest profile tumor types, such as breast, where HER2 testing drives therapeutic decisions. This review examines the area of tissue collection, transport, and monitoring of formalin diffusion and details a prototype system that could be used to help standardize tissue collection efforts. We have surveyed recent primary literature sources and conducted several site visits to understand the most error-prone processes in histology laboratories. This effort identified errors that resulted from sample collection techniques and subsequent transport delays from the operating room (OR) to the histology laboratories. We have therefore devised a prototype sample collection and transport concept. The system consists of a custom data logger and cold transport box and takes advantage of a novel cold + warm (named 2 + 2) fixation method. This review highlights the beneficial aspects of standardizing tissue collection, fixation, and monitoring. In addition, a prototype system is introduced that could help standardize these processes and is compatible with use directly in the OR and from remote sites.

Investigation on the performance of polymer zirconium compound (PZC) for chromatographic Tc-99m generator preparation

International Nuclear Information System (INIS)

Le Van So

2004-01-01

The performance of PZC was investigated for chromatographic Tc-99m generator preparation. Mo-adsorption of PZC in different Mo-solutions and Tc-99m elution of 99 Mo-PZC column were studied. Mo- adsorption capacity of higher than 250mgMo/gPZC and Tc-99m elution yield of higher than 80% were achieved with PZC adsorbent. Mo-99 breakthrough of 0.02% and Molybdenum element breakthrough of around 5μg Mo/ml were found in Tc-99m eluate. A good relationship between the Mo-content of adsorption solution and the Mo-adsorption capacity, adsorption percentage, Mo-breakthrough and Tc-99m elution yield was found. The preparation of PZC based Tc-99m chromatographic generator with 4 gram weight of PZC was successfully conducted. (author)

Reversed phase chromatographic behaviour of Pu (III), Pu (IV) and Pu (VI) in presence of α-hydroxyisobutyric acid

International Nuclear Information System (INIS)

Jaison, P.G.; Telmore, V.M.; Kumar, Pranaw

2016-01-01

Understanding the aqueous chemistry of plutonium is important in process conditions as well as in environmental conditions. Since plutonium possesses multiple oxidation states which can coexist in solution, a reliable method for the identification of these oxidation states is essential to understand its physical and chemical processes. The identification of plutonium oxidation states is conventionally determined through a series of liquid-liquid extraction procedures using selective extractants. Spectroscopic and laser based techniques also have been used for the identification of its oxidation state in solutions. Liquid chromatographic behavior of different oxidation states of Pu and other actinide ions is reported to correlate their retention behaviour with stability constants. Objective of the present work is to study the reversed phase chromatography behavior of the three oxidation states of plutonium viz. Pu(III), Pu(IV) and Pu(VI) in presence of á-hydroxyisobutyric acid (HIBA) as an eluent

Certification of selected polynuclear aromatic hydrocarbons in standard reference material 1580, 'Organics in Shale Oil'. Final report

Energy Technology Data Exchange (ETDEWEB)

May, W.E.; Brown-Thomas, J.M.; Hilpert, L.R.; Wise, S.A.

1981-01-01

Two independent analytical methods were developed and used to certify the concentrations of five polynuclear aromatic hydrocarbons (PAH) in a shale oil sample (SRM 1580). In the sequential high-performance liquid chromatographic method, PAH are isolated from the matrix by chromatography on an aminosilane column. The individual analyte species were separated, identified, and quantified by chromatography on an octadecylsilane column with spectrofluorimetric detection. Dilution of the sample in methylene chloride was the only sample preparation step necessary prior to analysis by gas chromatography/mass spectrometry (GC/MS). The GC/MS determinations were performed using selected ion monitoring (SIM) and a standard addition technique for quantification. The polynuclear aromatic hydrocarbons of interest were separated on a 30 m SE-52 wall coated open tubular column interfaced to a quadrupole mass spectrometer through a 25 cm length of Pt/Ir tubing (0.15 mm i.d.). Excellent agreement was observed between the data obtained from these methods.

[Standardization of Blastocystis hominis diagnosis using different staining techniques].

Science.gov (United States)

Eymael, Dayane; Schuh, Graziela Maria; Tavares, Rejane Giacomelli

2010-01-01

The present study was carried out from March to May 2008, with the aim of evaluating the effectiveness of different techniques for diagnosing Blastocystis hominis in a sample of the population attended at the Biomedicine Laboratory of Feevale University, Novo Hamburgo, Rio Grande do Sul. On hundred feces samples from children and adults were evaluated. After collection, the samples were subjected to the techniques of spontaneous sedimentation (HPJ), sedimentation in formalin-ether (Ritchie) and staining by means of Gram and May-Grünwald-Giemsa (MGG). The presence of Blastocystis hominis was observed in 40 samples, when staining techniques were used (MGG and Gram), while sedimentation techniques were less efficient (32 positive samples using the Ritchie technique and 20 positive samples using the HPJ technique). Our results demonstrate that HPJ was less efficient than the other methods, thus indicating the need to include laboratory techniques that enable parasite identification on a routine basis.

Lightening protection, techniques, applied codes and standards. Vol. 4

International Nuclear Information System (INIS)

Mahmoud, M.; Shaaban, H.; Lamey, S.

1996-01-01

Lightening is the only natural disaster that protection against is highly effective. Therefore for the safety of critical installations specifically nuclear, an effective lightening protection system (LPS) is required. The design and installation of LPS's have been addressed by many international codes and standards. In this paper, the various LPS's are discussed and compared, including radioactive air terminals, ionizing air terminals, and terminals equipped with electrical trigging devices. Also, the so-called dissipation array systems are discussed and compared to other systems technically and economically. Moreover, the available international codes and standards related to the lightening protection are discussed. such standards include those published by the national fire protection association (NFPA), lightening protection institute (LPI), underwriters laboratories (UL), and british standards Finally, the possibility of developing an egyptian national standards is discussed

Closing the gap: accelerating the translational process in nanomedicine by proposing standardized characterization techniques.

Science.gov (United States)

Khorasani, Ali A; Weaver, James L; Salvador-Morales, Carolina

2014-01-01

On the cusp of widespread permeation of nanomedicine, academia, industry, and government have invested substantial financial resources in developing new ways to better treat diseases. Materials have unique physical and chemical properties at the nanoscale compared with their bulk or small-molecule analogs. These unique properties have been greatly advantageous in providing innovative solutions for medical treatments at the bench level. However, nanomedicine research has not yet fully permeated the clinical setting because of several limitations. Among these limitations are the lack of universal standards for characterizing nanomaterials and the limited knowledge that we possess regarding the interactions between nanomaterials and biological entities such as proteins. In this review, we report on recent developments in the characterization of nanomaterials as well as the newest information about the interactions between nanomaterials and proteins in the human body. We propose a standard set of techniques for universal characterization of nanomaterials. We also address relevant regulatory issues involved in the translational process for the development of drug molecules and drug delivery systems. Adherence and refinement of a universal standard in nanomaterial characterization as well as the acquisition of a deeper understanding of nanomaterials and proteins will likely accelerate the use of nanomedicine in common practice to a great extent.

Chromatographic analysis of toxic phosphylated oximes (POX): a brief overview.

Science.gov (United States)

Becker, Christian; Worek, Franz; John, Harald

2010-10-01

Poisoning with organophosphorus compounds (OP), e.g. pesticides and nerve agents, causes inhibition of acetylcholinesterase (AChE) by phosphylation of the active site serine residue. Consequently, accumulation of stimulating acetylcholine in the synaptic cleft induces cholinergic crisis which ultimately may lead to death. For standard causal therapy, enzyme reactivators are administered representing oxime derivatives of quarternary pyridinium compounds, e.g. pralidoxime (2-PAM), obidoxime and HI 6. The mechanism of action includes removal of the phosphyl moiety by a nucleophilic attack of the oximate molecule substituting the enzyme and forming a phosphylated oxime (POX). POX is produced in stoichiometric amounts of reactivated enzyme and exhibits a significantly enhanced toxicity (inhibition rate constant) when compared to the parent OP. However, stability of POX under physiological conditions appears to be highly limited. Nevertheless, the presence of POX reveals a potential critical issue for both therapeutic efficacy in vivo and pharmacokinetic and pharmacodynamic (PK-PD) modelling based on cholinesterase activity data. Detailed characterization represents an important need for elaboration of the entire oxime pharmacology.Nevertheless, reports on POX toxicity and analysis are quite rare and may therefore be indicative of the challenge of POX analysis. This review provides a concise overview of chromatographic approaches applied to POX separation. Chromatography represents the key technology for POX purification and quantification in kinetic in vitro studies using buffers and biological fluids. Applications based on reversed-phase chromatography (RPC), ion pair chromatography (IPC) and an affinity approach as well as thin layer chromatography (TLC) are discussed and novel applications and data are presented. Copyright © 2010 John Wiley & Sons, Ltd.

Sample preparation for large-scale bioanalytical studies based on liquid chromatographic techniques.

Science.gov (United States)

Medvedovici, Andrei; Bacalum, Elena; David, Victor

2018-01-01

Quality of the analytical data obtained for large-scale and long term bioanalytical studies based on liquid chromatography depends on a number of experimental factors including the choice of sample preparation method. This review discusses this tedious part of bioanalytical studies, applied to large-scale samples and using liquid chromatography coupled with different detector types as core analytical technique. The main sample preparation methods included in this paper are protein precipitation, liquid-liquid extraction, solid-phase extraction, derivatization and their versions. They are discussed by analytical performances, fields of applications, advantages and disadvantages. The cited literature covers mainly the analytical achievements during the last decade, although several previous papers became more valuable in time and they are included in this review. Copyright © 2017 John Wiley & Sons, Ltd.

Radioimmunoassay and liquid-chromatographic analysis for free cortisol in urine compared with isotope dilution-mass spectrometry

International Nuclear Information System (INIS)

Lantto, O.

1982-01-01

Three different routine methods for analysis for urinary cortisol with those by a highly specific reference method based on isotope dilution-mass spectrometry (I) were compared. A ''high-performance'' liquid-chromatographic method (II) gave the most comparable results (regression coefficient 0.86, intercept 9 nmol/L). For some urines much lower values were obtained by I than by II. Two radioimmunoassay (III) methods, one involving direct assay and one involving extraction, gave less-accurate results (regression coefficients of 1.87 and 1.52 and intercepts of 86 and 12 nmol/L, respectively), although values obtained by III and by I correlated well (r = 0.95-0.99), indicating a relation between the free cortisol and the compounds interfering in III. The apparent accuracy for the extraction method was improved by using as calibration standards urine samples previously assayed by I (regression coefficient 0.90, intercept 6 nmol/L). All four methods investigated showed a statistically significant sex-related difference in 24-h urinary cortisol excretion; evidently such a finding should be a prerequisite in any such method proposed for routine use

Separation of rare earth by column chromatography using organic resins XAD/DEPHA

Energy Technology Data Exchange (ETDEWEB)

Zini, J.; Ferreira, J.C.; Bergamaschi, V.S.; Santos, I.; Carvalho, F.M.S., E-mail: jcferrei@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (CCCH/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Celulas a Combustivel e Hidrogenio

2013-07-01

The designation of light and heavy rare earth was used the fractionation used in separation processes. In this study the process of separation of rare earth, in groups, by chromatographic column consisting in fixing of cations these elements in an organic resin Amberlite XAD16 functionalized with the extracting agent DEPHA and another portion functionalized with a mixture of extractors DEPHA/TOP. The preparation of these resins was performed in two forms, one directly as the extracting agent to the resin and the other to be used in ethyl alcohol. Conditioned resins were introduced in chromatographic columns in separation of groups, light and heavy, using a standard solution of cerium nitrate and standard solution of holmium nitrate groups to represent light and heavy respectively. The characterization technique used to identify the rare earth elements was Spectrometry X-Ray Fluorescence (XRF). The results using the technique of chromatography were satisfactory, obtaining 100% separation of the elements. (author)

Separation of rare earth by column chromatography using organic resins XAD/DEPHA

International Nuclear Information System (INIS)

Zini, J.; Ferreira, J.C.; Bergamaschi, V.S.; Santos, I.; Carvalho, F.M.S.

2013-01-01

The designation of light and heavy rare earth was used the fractionation used in separation processes. In this study the process of separation of rare earth, in groups, by chromatographic column consisting in fixing of cations these elements in an organic resin Amberlite XAD16 functionalized with the extracting agent DEPHA and another portion functionalized with a mixture of extractors DEPHA/TOP. The preparation of these resins was performed in two forms, one directly as the extracting agent to the resin and the other to be used in ethyl alcohol. Conditioned resins were introduced in chromatographic columns in separation of groups, light and heavy, using a standard solution of cerium nitrate and standard solution of holmium nitrate groups to represent light and heavy respectively. The characterization technique used to identify the rare earth elements was Spectrometry X-Ray Fluorescence (XRF). The results using the technique of chromatography were satisfactory, obtaining 100% separation of the elements. (author)

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis.

Science.gov (United States)

Kshirsagar, Parthraj R; Hegde, Harsha; Pai, Sandeep R

2016-05-01

This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at -4°C. Contaminant peak was detected in methanol stored in polypropylene microcentrifuge tubes using UFLC analysis. The contaminant peak detected was prominent, sharp detectable at 9.176 ± 0.138 min on a Waters 250-4.6 mm, 4 μ, Nova-Pak C18 column with mobile phase consisting of methanol:water (70:30). It was evident from the study that long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peak. Further, this may mislead in future reporting an unnatural compound by researchers. Long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peakContamination peak with higher area under the curve (609993) was obtained in ultra-flow liquid chromatographic run for methanol stored in PP microcentrifuge tubesContamination peak was detected at retention time 9.113 min with a lambda max of 220.38 nm and 300 mAU intensity on the given chromatographic conditionsGlass vials serve better option over PP microcentrifuge tubes for storing biological samples. Abbreviations used: UFLC: Ultra Flow Liquid Chromatography; LC: Liquid Chromatography; MS: Mass spectrometry; AUC: Area Under Curve.

Strain analysis in CRT candidates using the novel segment length in cine (SLICE) post-processing technique on standard CMR cine images.

Science.gov (United States)

Zweerink, Alwin; Allaart, Cornelis P; Kuijer, Joost P A; Wu, LiNa; Beek, Aernout M; van de Ven, Peter M; Meine, Mathias; Croisille, Pierre; Clarysse, Patrick; van Rossum, Albert C; Nijveldt, Robin

2017-12-01

Although myocardial strain analysis is a potential tool to improve patient selection for cardiac resynchronization therapy (CRT), there is currently no validated clinical approach to derive segmental strains. We evaluated the novel segment length in cine (SLICE) technique to derive segmental strains from standard cardiovascular MR (CMR) cine images in CRT candidates. Twenty-seven patients with left bundle branch block underwent CMR examination including cine imaging and myocardial tagging (CMR-TAG). SLICE was performed by measuring segment length between anatomical landmarks throughout all phases on short-axis cines. This measure of frame-to-frame segment length change was compared to CMR-TAG circumferential strain measurements. Subsequently, conventional markers of CRT response were calculated. Segmental strains showed good to excellent agreement between SLICE and CMR-TAG (septum strain, intraclass correlation coefficient (ICC) 0.76; lateral wall strain, ICC 0.66). Conventional markers of CRT response also showed close agreement between both methods (ICC 0.61-0.78). Reproducibility of SLICE was excellent for intra-observer testing (all ICC ≥0.76) and good for interobserver testing (all ICC ≥0.61). The novel SLICE post-processing technique on standard CMR cine images offers both accurate and robust segmental strain measures compared to the 'gold standard' CMR-TAG technique, and has the advantage of being widely available. • Myocardial strain analysis could potentially improve patient selection for CRT. • Currently a well validated clinical approach to derive segmental strains is lacking. • The novel SLICE technique derives segmental strains from standard CMR cine images. • SLICE-derived strain markers of CRT response showed close agreement with CMR-TAG. • Future studies will focus on the prognostic value of SLICE in CRT candidates.

Comparison of multiple linear regression, partial least squares and artificial neural networks for prediction of gas chromatographic relative retention times of trimethylsilylated anabolic androgenic steroids.

Science.gov (United States)

Fragkaki, A G; Farmaki, E; Thomaidis, N; Tsantili-Kakoulidou, A; Angelis, Y S; Koupparis, M; Georgakopoulos, C

2012-09-21

The comparison among different modelling techniques, such as multiple linear regression, partial least squares and artificial neural networks, has been performed in order to construct and evaluate models for prediction of gas chromatographic relative retention times of trimethylsilylated anabolic androgenic steroids. The performance of the quantitative structure-retention relationship study, using the multiple linear regression and partial least squares techniques, has been previously conducted. In the present study, artificial neural networks models were constructed and used for the prediction of relative retention times of anabolic androgenic steroids, while their efficiency is compared with that of the models derived from the multiple linear regression and partial least squares techniques. For overall ranking of the models, a novel procedure [Trends Anal. Chem. 29 (2010) 101-109] based on sum of ranking differences was applied, which permits the best model to be selected. The suggested models are considered useful for the estimation of relative retention times of designer steroids for which no analytical data are available. Copyright © 2012 Elsevier B.V. All rights reserved.

Fuels characterization studies. [jet fuels

Science.gov (United States)

Seng, G. T.; Antoine, A. C.; Flores, F. J.

1980-01-01

Current analytical techniques used in the characterization of broadened properties fuels are briefly described. Included are liquid chromatography, gas chromatography, and nuclear magnetic resonance spectroscopy. High performance liquid chromatographic ground-type methods development is being approached from several directions, including aromatic fraction standards development and the elimination of standards through removal or partial removal of the alkene and aromatic fractions or through the use of whole fuel refractive index values. More sensitive methods for alkene determinations using an ultraviolet-visible detector are also being pursued. Some of the more successful gas chromatographic physical property determinations for petroleum derived fuels are the distillation curve (simulated distillation), heat of combustion, hydrogen content, API gravity, viscosity, flash point, and (to a lesser extent) freezing point.

Chromatographic assay of degradation products of tributyl phosphate

International Nuclear Information System (INIS)

Tripathi, S.C.; Ramanujam, A.; Nadkarni, M.N.; Rao, K.A.; Bandyopadhyay, C.

1985-01-01

Gas-liquid chromatography (GLC) and thin-layer chromatographic (TLC) procedures have been developed for the estimation of monobutyl phosphoric acid (H 2 MBP) and dibutyl phosphoric acid (HDBP) present in tributyl phosphate (TBP). Less than one microgram of H 2 MBP and HDBP is visually detected on TLC plate made of silicagel-cellulose (1:1). HDBP as separated by TLC has been quantitatively estimated in the range of 40-260 μg using an indirect spectrophotometric method. GLC method using 10 percent (W/W) XE-60 column can be effectively used for the simultaneous determination of 0.25 percent W/V H 2 MBP and HDBP present in 30 percent TBP-n-dodecane. The sensitivity may be enhanced 100 fold by careful column conditioning and judicious control of operational parameters. (author)

Mass-fragmentographic determination of 25-hydroxy-vitamin D3 using deuterium labeled internal standard

International Nuclear Information System (INIS)

Bjorkhem, I.; Holmberg, I.

1975-01-01

25-[26- 2 H 3 ] Hydroxy-vitamin D 3 has been synthesized according to the following route: 3β-acetoxy-27-nor-cholest-5-en-25-one → 3β-acetoxy-27-nor-cholesta-5,7-dien-25-one → [26- 2 H 3 ] cholesta-5,7-diene-3β,25-diol → 25-[26- 2 H 3 ] hydroxy-vitamin D 3 . A fixed amount of 25-[26- 2 H 3 ] hydroxy-vitamin D 3 , usually 250 ng, is added to a fixed amount of serum, usually 2.5 ml, and the mixture is extracted with a chloroform-methanol mixture. The extract is chromatographed on a Sephadex LH-20 column together with a trace amount of 25-[26- 3 H] hydroxy-vitamin D 3 . The chromatographic fraction corresponding to 25-hydroxy-vitamin D 3 is collected and the amount of unlabeled 25-hydroxy-vitamin D 3 is determined from the ratio between the mass fragmentographic recording of m/e 131 (base peak of unlabeled 25-hydroxy-vitamin D 3 ) and m/e 134 (base peak of 25-[26- 2 H 3 ] hydroxy-vitamin D 3 ). The relative standard deviation of the method was about 5%. The mean value for 25-hydroxy-vitamin D 3 obtained from 23 different serum samples from healthy Swedish men and women was 27 ng/ml with a standard deviation of 10 ng/ml

Optimisation of chromatographic resolution using objective functions including both time and spectral information.

Science.gov (United States)

Torres-Lapasió, J R; Pous-Torres, S; Ortiz-Bolsico, C; García-Alvarez-Coque, M C

2015-01-16

The optimisation of the resolution in high-performance liquid chromatography is traditionally performed attending only to the time information. However, even in the optimal conditions, some peak pairs may remain unresolved. Such incomplete resolution can be still accomplished by deconvolution, which can be carried out with more guarantees of success by including spectral information. In this work, two-way chromatographic objective functions (COFs) that incorporate both time and spectral information were tested, based on the peak purity (analyte peak fraction free of overlapping) and the multivariate selectivity (figure of merit derived from the net analyte signal) concepts. These COFs are sensitive to situations where the components that coelute in a mixture show some spectral differences. Therefore, they are useful to find out experimental conditions where the spectrochromatograms can be recovered by deconvolution. Two-way multivariate selectivity yielded the best performance and was applied to the separation using diode-array detection of a mixture of 25 phenolic compounds, which remained unresolved in the chromatographic order using linear and multi-linear gradients of acetonitrile-water. Peak deconvolution was carried out using the combination of orthogonal projection approach and alternating least squares. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid on-site sensing aflatoxin B1 in food and feed via a chromatographic time-resolved fluoroimmunoassay.

Directory of Open Access Journals (Sweden)

Zhaowei Zhang

Full Text Available Aflatoxin B1 poses grave threats to food and feed safety due to its strong carcinogenesis and toxicity, thus requiring ultrasensitive rapid on-site determination. Herein, a portable immunosensor based on chromatographic time-resolved fluoroimmunoassay was developed for sensitive and on-site determination of aflatoxin B1 in food and feed samples. Chromatographic time-resolved fluoroimmunoassay offered a magnified positive signal and low signal-to-noise ratio in time-resolved mode due to the absence of noise interference caused by excitation light sources. Compared with the immunosensing performance in previous studies, this platform demonstrated a wider dynamic range of 0.2-60 μg/kg, lower limit of detection from 0.06 to 0.12 µg/kg, and considerable recovery from 80.5% to 116.7% for different food and feed sample matrices. It was found to be little cross-reactivity with other aflatoxins (B2, G1, G2, and M1. In the case of determination of aflatoxin B1 in peanuts, corn, soy sauce, vegetable oil, and mouse feed, excellent agreement was found when compared with aflatoxin B1 determination via the conversational high-performance liquid chromatography method. The chromatographic time-resolved fluoroimmunoassay affords a powerful alternative for rapid on-site determination of aflatoxin B1 and holds a promise for food safety in consideration of practical food safety and environmental monitoring.

Rapid on-site sensing aflatoxin B1 in food and feed via a chromatographic time-resolved fluoroimmunoassay.

Science.gov (United States)

Zhang, Zhaowei; Tang, Xiaoqian; Wang, Du; Zhang, Qi; Li, Peiwu; Ding, Xiaoxia

2015-01-01

Aflatoxin B1 poses grave threats to food and feed safety due to its strong carcinogenesis and toxicity, thus requiring ultrasensitive rapid on-site determination. Herein, a portable immunosensor based on chromatographic time-resolved fluoroimmunoassay was developed for sensitive and on-site determination of aflatoxin B1 in food and feed samples. Chromatographic time-resolved fluoroimmunoassay offered a magnified positive signal and low signal-to-noise ratio in time-resolved mode due to the absence of noise interference caused by excitation light sources. Compared with the immunosensing performance in previous studies, this platform demonstrated a wider dynamic range of 0.2-60 μg/kg, lower limit of detection from 0.06 to 0.12 µg/kg, and considerable recovery from 80.5% to 116.7% for different food and feed sample matrices. It was found to be little cross-reactivity with other aflatoxins (B2, G1, G2, and M1). In the case of determination of aflatoxin B1 in peanuts, corn, soy sauce, vegetable oil, and mouse feed, excellent agreement was found when compared with aflatoxin B1 determination via the conversational high-performance liquid chromatography method. The chromatographic time-resolved fluoroimmunoassay affords a powerful alternative for rapid on-site determination of aflatoxin B1 and holds a promise for food safety in consideration of practical food safety and environmental monitoring.

Chromatographic analysis of methylglyoxal and other α-dicarbonyls using gas-diffusion microextraction.

Science.gov (United States)

Santos, Christiane M; Valente, Inês M; Gonçalves, Luís M; Rodrigues, José A

2013-12-07

Many α-dicarbonyl compounds such as methylglyoxal, diacetyl and pentane-2,3-dione are important quality markers of processed foods. They are produced by enzymatic and chemical processes, the Maillard reaction is the most known chemical route for α-dicarbonyl formation. In the case of methylglyoxal, there are obstacles to be overcome when analysing this compound due to its high reactivity, low volatility and low concentration. The use of extraction techniques based on the volatilization of methylglyoxal (like solid-phase microextraction) showed to be ineffective for the methylglyoxal extraction from aqueous solutions. Therefore, derivatization is typically applied to increase analyte's volatility. In this work a new methodology for the extraction and analysis of methylglyoxal and also diacetyl and pentane-2,3-dione from selected food matrices is presented. It is based on a gas-diffusion microextraction step followed by high performance liquid chromatographic analysis. It was successfully applied to port wines, black tea and soy sauce. Methylglyoxal, diacetyl and pentane-2,3-dione were quantified in the following concentration ranges: 0.24-1.74 mg L(-1), 0.1-1.85 mg L(-1) and 0.023-0.15 mg L(-1), respectively. The main advantages over existing methodologies are its simplicity in terms of sample handling, not requiring any chemical modification of the α-dicarbonyls prior to the extraction, low reagent consumption and short time of analysis.

Optimization, validation and standardization of a method of measuring the radiochemical purity of 99mTc-HMDP in Necker hospital

International Nuclear Information System (INIS)

Dumont, A.; Izembart, M.; Barritault, L.

1997-01-01

By the end of 1996, the tests of the radiochemical purity (RCP) of preparation of HMDP- 99m Tc at Necker hospital were effected by means of 'Tech-Kit' technique which allowed making evident only one radiochemical impurity, the free TcO 4 - . So, the aim of this work has been the search for another technique able to detect also the reduced hydrolyzed 99m Tc, and then, to optimize, validate and standardize this new technique. Several methods have been tested and compared on different points (the chemical species identified, practical difficulties, duration, reproducibility) in order to chose 'the best' one, consisting in associating two TLC (migration time, 3 minutes): - TLC no.1, ITLC-SG/Methyl-ethyl-ketone; - TLC no.2, ITLC-SG/1M Sodium acetate. This method has been subsequently: - optimized, concerning the quantity of deposed sampling, way of deposit drying, migration range, reading protocol by radio-chromatograph; - validated, by verifying the migration of radiochemical impurities by means of controls and by evaluating its sensitivity; - standardized, by defining the interest zones for interpreting the radio-chromatograms, by evaluating the reproducibility and by calculating the 'normal values' of RCP percentages. This method has been adopted as routine and with current recoil (40 preparations) and our conditions of realizations, the extreme values of the percentages obtained for the impurity zones of interests, have been the following: - TcO 4 - zone, [0.39%-1.07%]; - hydrolyzed reduced Tc zone, [0.96%-5.09%]. By taking into account their distribution we calculated a minimum RCP value of 94% to accept the preparation (the RCP being defined as equal to 100% - % TcO 4 - % hydrolyzed reduced Tc)

NET European Network on Neutron Techniques Standardization for Structural Integrity

International Nuclear Information System (INIS)

Youtsos, A.

2004-01-01

Improved performance and safety of European energy production systems is essential for providing safe, clean and inexpensive electricity to the citizens of the enlarged EU. The state of the art in assessing internal stresses, micro-structure and defects in welded nuclear components -as well as their evolution due to complex thermo-mechanical loads and irradiation exposure -needs to be improved before relevant structural integrity assessment code requirements can safely become less conservative. This is valid for both experimental characterization techniques and predictive numerical algorithms. In the course of the last two decades neutron methods have proven to be excellent means for providing valuable information required in structural integrity assessment of advanced engineering applications. However, the European industry is hampered from broadly using neutron research due to lack of harmonised and standardized testing methods. 35 European major industrial and research/academic organizations have joined forces, under JRC coordination, to launch the NET European Network on Neutron Techniques Standardization for Structural Integrity in May 2002. The NET collaborative research initiative aims at further development and harmonisation of neutron scattering methods, in support of structural integrity assessment. This is pursued through a number of testing round robin campaigns on neutron diffraction and small angle neutron scattering - SANS and supported by data provided by other more conventional destructive and non-destructive methods, such as X-ray diffraction and deep and surface hole drilling. NET also strives to develop more reliable and harmonized simulation procedures for the prediction of residual stress and damage in steel welded power plant components. This is pursued through a number of computational round robin campaigns based on advanced FEM techniques, and on reliable data obtained by such novel and harmonized experimental methods. The final goal of

Modification of ion chromatograph for analyses of radioactive samples

International Nuclear Information System (INIS)

Curfman, L.L.; Johnson, S.J.

1979-01-01

In ion chromatographic analysis, the sample is injected through a sample loop onto an analytical column where separation occurs. The sample then passes through a suppressor column to remove or neutralize background ions. A flow-through conductivity cell is used as a detector. Depending upon column and eluent selection, ion chromatography can be used for anion or cation analyses. Ion chromatography has proven to be a versatile analytical tool for the analysis of anions in Hanford waste samples. These radioactive samples range from caustic high salt solutions to hydrochloric acid dissolutions of insoluble sludges. Instrument modifications which provide safe and convenient handling of these samples without lengthening analysis time or altering instrument performance are described

Gas chromatographic/mass spectrometric determination of carbon isotope composition in unpurified samples: methamphetamine example.

Science.gov (United States)

Low, I A; Liu, R H; Legendre, M G; Piotrowski, E G; Furner, R L

1986-10-01

A gas chromatograph/quadrupole mass spectrometer system, operated in electron impact/selected ion monitoring mode, is used to determine the intensity ratio of the m/z 59 and the m/z 58 ions of the [C3H8N]+ fragment derived from methamphetamine samples synthesized with varying amounts of 13C-labeled methylamine. Crude products are introduced into the gas chromatograph without prior cleanup. The ratios measured were in excellent agreement with those calculated. A change in 0.25% use of 13C-methylamine is sufficient for product differentiation. The feasibility of using isotope labeling and subsequent mass spectrometric isotope ratio measurement as the basis of a compound tracing mechanism is discussed. Specifically, if methamphetamine samples manufactured from legal sources are asked to incorporate distinct 13C compositions, their sources can be traced when samples are diverted into illegal channels. Samples derived from illicit preparations can also be traced if the manufacturers of a precursor (methylamine in this case) incorporate distinct 13C compositions in their products.

Analysis of Sidestream Smoke VOCs and Characterization of their Odor Profiles by VOC Preconcentrator-GC-O Techniques

Directory of Open Access Journals (Sweden)

Higashi N

2014-12-01

Full Text Available Various techniques have been employed in the analysis of volatile organic compounds (VOCs. However, these techniques are insufficient for the precise analysis of tobacco smoke VOCs because of the complexity of the operating system, system instability, or poor sensitivity. To overcome these problems, a combined system of VOC preconcentrator, gas chromatograph, and olfactometer has been developed. The performance of this new system was evaluated in the analysis of VOCs in tobacco smoke and applied to the odor profiling of sidestream smoke (SSS that has not been sufficiently investigated in the past.

Techniques for Analysis of Plant Phenolic Compounds

Directory of Open Access Journals (Sweden)

Thomas H. Roberts

2013-02-01

Full Text Available Phenolic compounds are well-known phytochemicals found in all plants. They consist of simple phenols, benzoic and cinnamic acid, coumarins, tannins, lignins, lignans and flavonoids. Substantial developments in research focused on the extraction, identification and quantification of phenolic compounds as medicinal and/or dietary molecules have occurred over the last 25 years. Organic solvent extraction is the main method used to extract phenolics. Chemical procedures are used to detect the presence of total phenolics, while spectrophotometric and chromatographic techniques are utilized to identify and quantify individual phenolic compounds. This review addresses the application of different methodologies utilized in the analysis of phenolic compounds in plant-based products, including recent technical developments in the quantification of phenolics.

EUS-guided biliary drainage by using a standardized approach for malignant biliary obstruction: rendezvous versus direct transluminal techniques (with videos).

Science.gov (United States)

Khashab, Mouen A; Valeshabad, Ali Kord; Modayil, Rani; Widmer, Jessica; Saxena, Payal; Idrees, Mehak; Iqbal, Shahzad; Kalloo, Anthony N; Stavropoulos, Stavros N

2013-11-01

EUS-guided biliary drainage (EGBD) can be performed via direct transluminal or rendezvous techniques. It is unknown how both techniques compare in terms of efficacy and adverse events. To describe outcomes of EGBD performed by using a standardized approach and compare outcomes of rendezvous and transluminal techniques. Retrospective analysis of prospectively collected data. Two tertiary-care centers. Consecutive jaundiced patients with distal malignant biliary obstruction who underwent EGBD after failed ERCP between July 2006 and December 2012 were included. EGBD by using a standardized algorithm. Technical success, clinical success, and adverse events. During the study period, 35 patients underwent EGBD (rendezvous n = 13, transluminal n = 20). Technical success was achieved in 33 patients (94%), and clinical success was attained in 32 of 33 patients (97.0%). The mean postprocedure bilirubin level was 1.38 mg/dL in the rendezvous group and 1.33 mg/dL in the transluminal group (P = .88). Similarly, length of hospital stay was not different between groups (P = .23). There was no significant difference in adverse event rate between rendezvous and transluminal groups (15.4% vs 10%; P = .64). Long-term outcomes were comparable between groups, with 1 stent migration in the rendezvous group at 62 days and 1 stent occlusion in the transluminal group at 42 days after EGBD. Retrospective analysis, small number of patients, and selection bias. EGBD is safe and effective when the described standardized approach is used. Stent occlusion is not common during long-term follow-up. Both rendezvous and direct transluminal techniques seem to be equally effective and safe. The latter approach is a reasonable alternative to rendezvous EGBD. Copyright © 2013. Published by Mosby, Inc.

Theory and practical understanding of the migration behavior of proteins and peptides in CE and related techniques.

Science.gov (United States)

Freitag, Ruth; Hilbrig, Frank

2007-07-01

CEC is defined as an analytical method, where the analytes are separated on a chromatographic column in the presence of an applied voltage. The separation of charged analytes in CEC is complex, since chromatographic interaction, electroosmosis and electrophoresis contribute to the experimentally observed behavior. The putative contribution of effects such as surface electrodiffusion has been suggested. A sound theoretical treatment incorporating all effects is currently not available. The question of whether the different effects contribute in an independent or an interdependent manner is still under discussion. In this contribution, the state-of-the-art in the theoretical description of the individual contributions as well as models for the retention behavior and in particular possible dimensionless 'retention factors' is discussed, together with the experimental database for the separation of charged analytes, in particular proteins and peptides, by CEC and related techniques.

Comparison of ankle-brachial index measured by an automated oscillometric apparatus with that by standard Doppler technique in vascular patients

DEFF Research Database (Denmark)

Korno, M.; Eldrup, N.; Sillesen, H.

2009-01-01

was calculated twice using both the methods on both legs. MATERIALS AND METHODS: We tested the automated oscillometric blood pressure device, CASMED 740, for measuring ankle and arm blood pressure and compared it with the current gold standard, the hand-held Doppler technique, by the Bland-Altman analysis....... RESULTS: Using the Doppler-derived ABI as the gold standard, the sensitivity and specificity of the oscillometric method for determining an ABI Udgivelsesdato: 2009/11...

Chromatographic speciation of Cr(III)-species, inter-species equilibrium isotope fractionation and improved chemical purification strategies for high-precision isotope analysis.

Science.gov (United States)

Larsen, K K; Wielandt, D; Schiller, M; Bizzarro, M

2016-04-22

Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of these species can result in incomplete Cr recovery during chromatographic purification. Because of large mass-dependent inter-species isotope fractionation, incomplete recovery can affect the accuracy of high-precision Cr isotope analysis. Here, we demonstrate widely differing cation distribution coefficients of Cr(III)-species (Cr(3+), CrCl(2+) and CrCl2(+)) with equilibrium mass-dependent isotope fractionation spanning a range of ∼1‰/amu and consistent with theory. The heaviest isotopes partition into Cr(3+), intermediates in CrCl(2+) and the lightest in CrCl2(+)/CrCl3°. Thus, for a typical reported loss of ∼25% Cr (in the form of Cr(3+)) through chromatographic purification, this translates into 185 ppm/amu offset in the stable Cr isotope ratio of the residual sample. Depending on the validity of the mass-bias correction during isotope analysis, this further results in artificial mass-independent effects in the mass-bias corrected (53)Cr/(52)Cr (μ(53)Cr* of 5.2 ppm) and (54)Cr/(52)Cr (μ(54)Cr* of 13.5 ppm) components used to infer chronometric and nucleosynthetic information in meteorites. To mitigate these fractionation effects, we developed strategic chemical sample pre-treatment procedures that ensure high and reproducible Cr recovery. This is achieved either through 1) effective promotion of Cr(3+) by >5 days exposure to HNO3H2O2 solutions at room temperature, resulting in >∼98% Cr recovery for most types of sample matrices tested using a cationic chromatographic retention strategy, or 2) formation of Cr(III)-Cl complexes through exposure to concentrated HCl at high temperature (>120 °C) for several hours, resulting in >97.5% Cr recovery using a

Wavelength standards in the infrared

CERN Document Server

Rao, KN

2012-01-01

Wavelength Standards in the Infrared is a compilation of wavelength standards suitable for use with high-resolution infrared spectrographs, including both emission and absorption standards. The book presents atomic line emission standards of argon, krypton, neon, and xenon. These atomic line emission standards are from the deliberations of Commission 14 of the International Astronomical Union, which is the recognized authority for such standards. The text also explains the techniques employed in determining spectral positions in the infrared. One of the techniques used includes the grating con

Multiple-channel ultra-violet absorbance detector for two-dimensional chromatographic separations.

Science.gov (United States)

Lynch, Kyle B; Yang, Yu; Ren, Jiangtao; Liu, Shaorong

2018-05-01

In recent years, much research has gone into developing online comprehensive two-dimensional liquid chromatographic systems allowing for high peak capacities in comparable separation times to that of one-dimensional liquid chromatographic systems. However, the speed requirements in the second dimension (2nd-D) still remain one challenge for complex biological samples due to the current configuration of two column/two detector systems. Utilization of multiple 2nd-D columns can mitigate this challenge. To adapt this approach, we need a multiple channel detector. Here we develop a versatile multichannel ultraviolet (UV) light absorbance detector that is capable of simultaneously monitoring separations in 12 columns. The detector consists of a deuterium lighthouse, a flow cell assembly (a 13-channel flow cell fitted with a 13-photodiode-detection system), and a data acquisition and monitoring terminal. Through the use of a custom high optical quality furcated fiber to improve light transmission, precise machining of a flow cell to reduce background stray light through precision alignment, and sensitive electronic circuitry to reduce electronic noise through an active low pass filter, the background noise level is measured in the tens of µAU. We obtain a linear dynamic range of close to three orders of magnitude. Compared to a commercialized multichannel UV light absorbance detector like the Waters 2488 UV/Vis, our device provides an increase in channel detection while residing within the same noise region and linear range. Copyright © 2018 Elsevier B.V. All rights reserved.

Volatilizable Biogenic Organic Compounds (VBOCs with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS: sampling methods, VBOC complexity, and chromatographic retention data

Directory of Open Access Journals (Sweden)

C. Chen

2012-02-01

Full Text Available Two dimensional gas chromatography (GC × GC with detection by time-of-flight mass spectrometry (TOFMS was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs. VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD cartridges and solid-phase microextraction (SPME fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film. Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m−3 for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m−3 for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and

Volatilizable Biogenic Organic Compounds (VBOCs) with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS): sampling methods, VBOC complexity, and chromatographic retention data

Science.gov (United States)

Pankow, J. F.; Luo, W.; Melnychenko, A. N.; Barsanti, K. C.; Isabelle, L. M.; Chen, C.; Guenther, A. B.; Rosenstiel, T. N.

2012-02-01

Two dimensional gas chromatography (GC × GC) with detection by time-of-flight mass spectrometry (TOFMS) was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs). VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD) cartridges and solid-phase microextraction (SPME) fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus) were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film) and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film). Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m-3) for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m-3) for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and other compounds

Single-column extraction chromatographic separation of U, Pu, Np and Am

Energy Technology Data Exchange (ETDEWEB)

Morgenstern, A.; Apostolidis, C.; Carlos-Marquez, R.; Mayer, K.; Molinet, R. [Commission of the European Communities, Karlsruhe (Germany). European Inst. for Transuranium Elements

2002-07-01

A rapid, single-column extraction chromatographic method using commercially available UTEVA resin has been developed for the separation of uranium, plutonium, neptunium and americium. The method yields recoveries superior to 90% and allows direct loading of separated fractions on filaments for subsequent analysis by thermal ionization mass spectrometry. The use of reagents compatible with robotized equipment allows automation of the separation process for routine analysis of nuclear materials. The redox reactions between plutonium, neptunium and hydrogen peroxide involved in the separation process were studied by UV/Vis/NIR absorption spectroscopy. (orig.)

Direct radioimmunoassay of proinsulin and insulin in human plasma by the chromatographic technique

Energy Technology Data Exchange (ETDEWEB)

Megahed, Y M; Abdel-Wahab, M F; El-Shawarbie, K; Sadek, S; Amer, M S [Atomic Energy Establishment, Cairo (Egypt). Radioisotope Department; Ain Shams Univ., Cairo (Egypt). Faculty of Medicine)

1976-04-01

Specific method for direct radioimmunoassay of IRP and IRI separately in human plasma has been described. The method is used for extraction of total insulin and separation of IRP from IRI by paper chromatography to be assayed separately. The separation of the two components is identified and confirmed by column chromatography, paper chromatography and ultraviolet spectral analysis in comparison with the standard compounds. 134 plasma samples of different cases were investigated for the determination of IRI, IRP and IRT. Out of these 39 were normals, 16 normal obes, 21 juvinil diabetes, 18 overt adult diabetes, 10 recent adult diabetes, 12 hypothyroidism and 18 bilharzial hepatosplenomegaly. They were used to evaluate the test levels in comparison with blood sugar concentration.

Characterization of used lubricating oil by spectrometric techniques

Energy Technology Data Exchange (ETDEWEB)

Souza, Andressa Moreira de, E-mail: andressa@ctaa.embrapa.br [Embrapa Agroindustria de Alimentos, Guaratiba, Rio de Janeiro, RJ (Brazil); Correa, Sergio Machado [Faculdade de Engenharia. Universidade do Estado do Rio de Janeiro (UERJ), Resende, RJ (Brazil); Silva, Glauco Correa da [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

2011-07-01

Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer{sup R} OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu{sup R} model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100{mu}A, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics

Characterization of used lubricating oil by spectrometric techniques

International Nuclear Information System (INIS)

Souza, Andressa Moreira de; Correa, Sergio Machado; Silva, Glauco Correa da

2011-01-01

Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer R OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu R model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

A rapid, solid phase extraction (SPE technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

Directory of Open Access Journals (Sweden)

Yuningsih

2006-03-01

Full Text Available Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk, so its become a problem in food safety. Solid phase extraction (SPE has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue and milk samples respectively. The recoveries of tissue sample by addition lindane standard solution: 0.50 and 1.00 μg are 85.10 and 103.10% respectively, while that of milk with the addition of 0.50, 1.00 and 1.50 μg are 83.80, 88.69 and 91.24% respectively. Three replicates were carried out for every sample. According of validation criteria of FAO/IAEA the recovery for analysis of pesticide residues was 70-110%. Therefore, the method is applicable.

Fuzzy clustering evaluation of the discrimination power of UV-Vis and (±) ESI-MS detection system in individual or coupled RPLC for characterization of Ginkgo Biloba standardized extracts.

Science.gov (United States)

Medvedovici, Andrei; Albu, Florin; Naşcu-Briciu, Rodica Domnica; Sârbu, Costel

2014-02-01

Discrimination power evaluation of UV-Vis and (±) electrospray ionization/mass spectrometric techniques, (ESI-MS) individually considered or coupled as detectors to reversed phase liquid chromatography (RPLC) in the characterization of Ginkgo Biloba standardized extracts, is used in herbal medicines and/or dietary supplements with the help of Fuzzy hierarchical clustering (FHC). Seventeen batches of Ginkgo Biloba commercially available standardized extracts from seven manufacturers were measured during experiments. All extracts were within the criteria of the official monograph dedicated to dried refined and quantified Ginkgo extracts, in the European Pharmacopoeia. UV-Vis and (±) ESI-MS spectra of the bulk standardized extracts in methanol were acquired. Additionally, an RPLC separation based on a simple gradient elution profile was applied to the standardized extracts. Detection was made through monitoring UV absorption at 220 nm wavelength or the total ion current (TIC) produced through (±) ESI-MS analysis. FHC was applied to raw, centered and scaled data sets, for evaluating the discrimination power of the method with respect to the origins of the extracts and to the batch to batch variability. The discrimination power increases with the increase of the intrinsic selectivity of the spectral technique being used: UV-Visstandardized extracts, and at some extent, to monitor the inter-batch variability. Although the chromatographic dimension sensibly contributes to the discrimination power, spectral MS data may be used as the lone powerful holistic alternative in characterization of standardized Ginkgo Biloba extracts. © 2013 Elsevier B

Creating New Technologists of Research in the 1960s: The Case of the Reproduction of Automated Chromatography Specialists and Practitioners

Science.gov (United States)

Gerontas, Apostolos

2014-01-01

Chromatographic instrumentation has been really influential in shaping the modern chemical practice, and yet it has been largely overlooked by history of science.Gas chromatography in the 1960s was considered the analytical technique closer to becoming dominant, and being the first automated chromatography set the standards that all the subsequent…

Chromatographic Separation of Vitamin E Enantiomers

Directory of Open Access Journals (Sweden)

Ju-Yen Fu

2017-02-01

Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

Using Aspen to Teach Chromatographic Bioprocessing: A Case Study in Weak Partitioning Chromatography for Biotechnology Applications

Science.gov (United States)

Evans, Steven T.; Huang, Xinqun; Cramer, Steven M.

2010-01-01

The commercial simulator Aspen Chromatography was employed to study and optimize an important new industrial separation process, weak partitioning chromatography. This case study on antibody purification was implemented in a chromatographic separations course. Parametric simulations were performed to investigate the effect of operating parameters…

Diffusion and flow of water vapours in chromatographic Alumina gel

International Nuclear Information System (INIS)

Khan, M.; Shah, H. U.

2005-01-01

The kinetics of sorption of water vapours in chromatographic alumina gel was studied. Water vapours are adsorbed on the gel at temperature (15 degree C) at different constant relative pressure from 0.1-0.93 p/p. Rate constant, Effective diffusivities, Knudsen diffusivities and bulk diffusivities were determined through Fick type equation. Total pore volume is 0.498 cc g-1 and specific surface area comes to be 465 m2 g-1 as obtained by Gurvitsch rule and Kieselve's quantities respectively. An average pore radius (hydraulic) is 1.1x10/sub -7/ cm. The study of these quantities provide a strong basis for evaluating surface properties. (author)

Strain analysis in CRT candidates using the novel segment length in cine (SLICE) post-processing technique on standard CMR cine images

Energy Technology Data Exchange (ETDEWEB)

Zweerink, Alwin; Allaart, Cornelis P.; Wu, LiNa; Beek, Aernout M.; Rossum, Albert C. van; Nijveldt, Robin [VU University Medical Center, Department of Cardiology, and Institute for Cardiovascular Research (ICaR-VU), Amsterdam (Netherlands); Kuijer, Joost P.A. [VU University Medical Center, Department of Physics and Medical Technology, Amsterdam (Netherlands); Ven, Peter M. van de [VU University Medical Center, Department of Epidemiology and Biostatistics, Amsterdam (Netherlands); Meine, Mathias [University Medical Center, Department of Cardiology, Utrecht (Netherlands); Croisille, Pierre; Clarysse, Patrick [Univ Lyon, UJM-Saint-Etienne, INSA, CNRS UMR 5520, INSERM U1206, CREATIS, Saint-Etienne (France)

2017-12-15

Although myocardial strain analysis is a potential tool to improve patient selection for cardiac resynchronization therapy (CRT), there is currently no validated clinical approach to derive segmental strains. We evaluated the novel segment length in cine (SLICE) technique to derive segmental strains from standard cardiovascular MR (CMR) cine images in CRT candidates. Twenty-seven patients with left bundle branch block underwent CMR examination including cine imaging and myocardial tagging (CMR-TAG). SLICE was performed by measuring segment length between anatomical landmarks throughout all phases on short-axis cines. This measure of frame-to-frame segment length change was compared to CMR-TAG circumferential strain measurements. Subsequently, conventional markers of CRT response were calculated. Segmental strains showed good to excellent agreement between SLICE and CMR-TAG (septum strain, intraclass correlation coefficient (ICC) 0.76; lateral wall strain, ICC 0.66). Conventional markers of CRT response also showed close agreement between both methods (ICC 0.61-0.78). Reproducibility of SLICE was excellent for intra-observer testing (all ICC ≥0.76) and good for interobserver testing (all ICC ≥0.61). The novel SLICE post-processing technique on standard CMR cine images offers both accurate and robust segmental strain measures compared to the 'gold standard' CMR-TAG technique, and has the advantage of being widely available. (orig.)

Strain analysis in CRT candidates using the novel segment length in cine (SLICE) post-processing technique on standard CMR cine images

International Nuclear Information System (INIS)

Zweerink, Alwin; Allaart, Cornelis P.; Wu, LiNa; Beek, Aernout M.; Rossum, Albert C. van; Nijveldt, Robin; Kuijer, Joost P.A.; Ven, Peter M. van de; Meine, Mathias; Croisille, Pierre; Clarysse, Patrick

2017-01-01

Although myocardial strain analysis is a potential tool to improve patient selection for cardiac resynchronization therapy (CRT), there is currently no validated clinical approach to derive segmental strains. We evaluated the novel segment length in cine (SLICE) technique to derive segmental strains from standard cardiovascular MR (CMR) cine images in CRT candidates. Twenty-seven patients with left bundle branch block underwent CMR examination including cine imaging and myocardial tagging (CMR-TAG). SLICE was performed by measuring segment length between anatomical landmarks throughout all phases on short-axis cines. This measure of frame-to-frame segment length change was compared to CMR-TAG circumferential strain measurements. Subsequently, conventional markers of CRT response were calculated. Segmental strains showed good to excellent agreement between SLICE and CMR-TAG (septum strain, intraclass correlation coefficient (ICC) 0.76; lateral wall strain, ICC 0.66). Conventional markers of CRT response also showed close agreement between both methods (ICC 0.61-0.78). Reproducibility of SLICE was excellent for intra-observer testing (all ICC ≥0.76) and good for interobserver testing (all ICC ≥0.61). The novel SLICE post-processing technique on standard CMR cine images offers both accurate and robust segmental strain measures compared to the 'gold standard' CMR-TAG technique, and has the advantage of being widely available. (orig.)

Selective micellar electrokinetic chromatographic method for simultaneous determination of some pharmaceutical binary mixtures containing non-steroidal anti-inflammatory drugs

Directory of Open Access Journals (Sweden)

Michael E. El-Kommos

2013-02-01

Full Text Available A simple and selective micellar electrokinetic chromatographic (MEKC method has been developed for the analysis of five pharmaceutical binary mixtures containing three non-steroidal anti-inflammatory drugs (NSAIDs. The investigated mixtures were Ibuprofen (IP–Paracetamol (PC, Ibuprofen (IP–Chlorzoxazone (CZ, Ibuprofen (IP–Methocarbamol (MC, Ketoprofen (KP–Chlorzoxazone (CZ and Diclofenac sodium (DS–Lidocaine hydrochloride (LC. The separation was run for all mixtures using borate buffer (20 mM, pH 9 containing 15% (v/v methanol and 100 mM sodium dodecyl sulphate (SDS at 15 kV and the components were detected at 214 nm. Different factors affecting the electrophoretic mobility of the seven investigated drugs were studied and optimized. The method was validated according to international conference of harmonization (ICH guidelines and United States pharmacopoeia (USP. The method was applied to the analysis of five pharmaceutical binary mixtures in their dosage forms. The results were compared with other reported high performance liquid chromatographic methods and no significant differences were observed. Keywords: Capillary electrophoresis, Micellar electrokinetic chromatographic method, Non-steroidal anti-inflammatory drugs, Pharmaceutical binary mixtures, Pharmaceutical analysis

Protein selectivity with immobilized metal ion-tacn sorbents: chromatographic studies with human serum proteins and several other globular proteins.

Science.gov (United States)

Jiang, W; Graham, B; Spiccia, L; Hearn, M T

1998-01-01

The chromatographic selectivity of the immobilized chelate system, 1,4,7-triazocyclononane (tacn), complexed with the borderline metal ions Cu2+, Cr3+, Mn2+, Co2+, Zn2+, and Ni2+ has been investigated with hen egg white lysozyme, horse heart cytochrome c, and horse skeletal muscle myoglobin, as well as proteins present in partially fractionated preparations of human plasma. The effects of ionic strength and pH of the loading and elution buffers on protein selectivities of these new immobilized metal ion affinity chromatographic (IMAC) systems have been examined. The results confirm that immobilized Mn;pl-tacn sorbents exhibit a novel type of IMAC behavior with proteins. In particular, the chromatographic properties of these immobilized M(n+)-tacn ligand systems were significantly different compared to the IMAC behavior observed with other types of immobilized tri- and tetradentate chelating ligands, such as iminodiacetic acid, O-phosphoserine, or nitrilotriacetic acid, when complexed with borderline metal ions. The experimental results have consequently been evaluated in terms of the additional contributions to the interactive processes mediated by effects other than solely the conventional lone pair Lewis soft acid-Lewis soft base coordination interactions, typically found for the IMAC of proteins with borderline and soft metal ions, such as Cu2+ or Ni2+.

Studies on Chromatographic Fingerprint and Fingerprinting Profile-Efficacy Relationship of Polygoni Perfoliati Herba

Directory of Open Access Journals (Sweden)

Li Tian

2013-01-01

Full Text Available Polygoni Perfoliati Herba is widely used in China with antibacterium, anti-inflammatory, expectorant, antitumor, and antivirus activities. To reveal the mechanisms of the activities of Polygoni Perfoliati Herba, the relationship between the fingerprinting profile and its bioactivities was investigated. In the present study, high-performance liquid chromatographic (HPLC fingerprinting method was developed. The established method was applied to analyze 51 batches of Polygoni Perfoliati Herba samples collected from different locations or in different harvesting times in China. Chemometrics, including similarity analysis, hierarchical clustering analysis, and principal component analysis, were used to express their similarities. It was found that similarity values of the samples were in the range of 0.432–0.998. The results of analgesic tests indicated that Polygoni Perfoliati Herba could significantly inhibit pain induced by hot plate and acetic acid in mice. The results of anti-inflammatory tests showed that Polygoni Perfoliati Herba had good anti-inflammatory effects (P < 0.01 in two models including dimethyl benzene-induced ear edema and acetic acid-induced peritoneal permeability in mice. Combining the results from chromatographic fingerprints with those from bioactivities, we found that seven peaks from Polygoni Perfoliati Herba were mainly responsible for analgesic and anti-inflammatory activities.

Chromatographic, Spectroscopic and Mass Spectrometric Approaches for Exploring the Habitability of Mars in 2012 and Beyond with the Curiosity Rover

Science.gov (United States)

Mahaffy, Paul

2012-01-01

The Sample Analysis at Mars (SAM) suite of instruments on the Curiosity Rover of Mars Science Laboratory Mission is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The goals of the science investigation enabled by the gas chromatograph mass spectrometer and tunable laser spectrometer instruments of SAM are to work together with the other MSL investigations is to quantitatively assess habitability through a series of chemical and geological measurements. We describe the multi-column gas chromatograph system employed on SAM and the approach to extraction and analysis of organic compounds that might be preserved in ancient martian rocks.

Selected Bibliography of the Nephrourology standard techniques

International Nuclear Information System (INIS)

1999-01-01

In the mark of the first meeting of project coordinators ARCAL XXXVI a selected Bibliography is presented about standardization of technical of Nuclear Nephrourology .In this selection it found: radiopharmaceuticals used, quality control,dosimetry, obstruction, clearance and renal function paediatric aspects pielonephritis,Renovascular hypertension and renal transplant [es

Liquid chromatographic determination with fluorescence detection of B6 vitamers and riboflavin in milk and pharmaceuticals

International Nuclear Information System (INIS)

Gatti, R.; Gioia, M.G.

2005-01-01

A simple, reliable and selective high performance liquid chromatographic method with fluorescence detection at different programmed wavelengths has been developed for the simultaneous analysis of B 6 vitamers (pyridoxal 5'-phosphate, 4-pyridoxic acid, pyridoxal, pyridoxine and pyridoxamine) and Vitamin B 2 in commercial vitaminized milk and in woman milk. The chromatographic separations were performed on a reversed phase octyl column by using a mobile phase consisting of sodium pentanesulfonate in 1% acetic acid-methanol-tetrahydrofuran under gradient elution conditions. The fluorescence intensity of pyridoxal 5'-phosphate was enhanced by post-column photochemical conversion, giving significantly different fluorescence spectra by a on-line photoreactor switched OFF and ON under irradiation at 254 nm. In addition, a simple and rapid method in isocratic conditions without the need of photochemical conversion was proposed for the analysis of Vitamin B 6 and Vitamin B 2 in pharmaceuticals. Linearity, precision, recovery, selectivity and sensitivity were found satisfactory for each analysed compound. Quantitation limits ranged from 26 to 240 fmol

Procedures for the production of poly-zirconium-compound (PZC) based chromatographic 99mTc generator to be available for clinical application

International Nuclear Information System (INIS)

Le Van So

2006-01-01

Two procedures - Column post-loading and Column pre-loading procedures - for the preparation of PZC based chromatographic Tc-99m generators were described in detail. In-process documentation, flow-chart of process for the individual procedures, specific Tc-99m generator designs and pictorially illustrative description of Tc-99m generator production process were systematically reported. The column pre-loading procedure was highly evaluated as a competent technology for the preparation of PZC based Tc-99m chromatographic generator of high performance using (n, γ) 99 Mo of low specific radioactivity produced on low power research reactors. (author)

Chromatographic retention of molybdenum, titanium and uranium complexes for removal of some interferences in inductively-coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Jiang, S.-J.; Palmieri, M.D.; Fritz, J.S.; Houk, R.S.; Iowa State Univ., of Science and Technology, Ames

1987-01-01

Complexes of molybdenum(VI) or titanium(IV) with N-methylfurohydroxamic acid (N-MFHA) are retained on a column packed with polystyrene/divinylbenzene. At the pH values chosen, copper, zinc and cadmium are washed rapidly through the column and are detected by inductively-coupled plasma mass spectrometry without interference from metal oxide ions of titanium or molybdenum. Detection limits are 1 to 2 μg l -1 , and analyte recoveries are essentially 100%. The resin capacity for the titanium and molybdenum complexes is sufficient for several hundred injections, and the complexes can be readily washed from the column. Uranium(VI) also forms a stable complex with N-MFHA, and ionization interference caused by excess of uranium can be avoided by chromatographic removal of the uranium complex. Various other potentially interfering elements with aqueous oxidation states of +4 or higher (e.g. Sn, W, Hf or Zr) could also be separated by this technique. 33 refs.; 4 figs.; 3 tabs

Measurement method for benzene, toluene, and xylene in the atmosphere by the gas chromatographic method

Energy Technology Data Exchange (ETDEWEB)

Shiroyama, H

1975-08-01

The chromatographic method for measuring benzene, toluene, and xylene (three isomers) in the atmosphere was evaluated using the Varian model 2740-10 gas chromatograph. As a solvent, n-hexane was most suitable, and the detection limit was improved by increasing the purity of n-hexane. The calibration curves were prepared, the recovery rate was calculated (76.0-99.4 percent), and the correlation coefficient was obtained from regression curves (r equals 0.97-0.99). Samples collected at a naphtha cracking plant, an aluminum smelting mill, a pharmaceutical plant, a carbon electrode manufacturing plant, a plywood manufacturing plant, a plastic bathtub manufacturing plant, and along a major highway were analyzed. All three substances were detected in all samples with the concentration of toluene high compared to the other two. Among xylene isomers, the concentration of p-xylene was always the lowest while m- and o-xylene varied from place to place. In the atmosphere along the highway, the benzene, toluene, and xylene determined were 0.01-0.09 ppM. No benzene, toluene, and xylene were detected in atmospheric samples used as controls.

Loop system for creating jet fuel vapor standards used in the calibration of infrared spectrophotometers and gas chromatographs.

Science.gov (United States)

Reboulet, James; Cunningham, Robert; Gunasekar, Palur G; Chapman, Gail D; Stevens, Sean C

2009-02-01

A whole body inhalation study of mixed jet fuel vapor and its aerosol necessitated the development of a method for preparing vapor only standards from the neat fuel. Jet fuel is a complex mixture of components which partitions between aerosol and vapor when aspirated based on relative volatility of the individual compounds. A method was desired which could separate the vapor portion from the aerosol component to prepare standards for the calibration of infrared spectrophotometers and a head space gas chromatography system. A re-circulating loop system was developed which provided vapor only standards whose composition matched those seen in an exposure system. Comparisons of nominal concentrations in the exposure system to those determined by infrared spectrophotometry were in 92-95% agreement. Comparison of jet fuel vapor concentrations determined by infrared spectrophotometry compared to head space gas chromatography yielded a 93% overall agreement in trial runs. These levels of agreement show the loop system to be a viable method for creating jet fuel vapor standards for calibrating instruments.

A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water.

Science.gov (United States)

Seiber, J N; Glotfelty, D E; Lucas, A D; McChesney, M M; Sagebiel, J C; Wehner, T A

1990-01-01

A multiresidue analytical method is described for pesticides, transformation products, and related toxicants based upon high performance liquid chromatographic (HPLC) fractionation of extracted residue on a Partisil silica gel normal phase column followed by selective-detector gas chromatographic (GC) determination of components in each fraction. The HPLC mobile phase gradient (hexane to methyl t-butyl ether) gave good chromatographic efficiency, resolution, reproducibility and recovery for 61 test compounds, and allowed for collection in four fractions spanning polarities from low polarity organochlorine compounds (fraction 1) to polar N-methylcarbamates and organophosphorus oxons (fraction 4). The multiresidue method was developed for use with air samples collected on XAD-4 and related trapping agents, and water samples extracted with methylene chloride. Detection limits estimated from spiking experiments were generally 0.3-1 ng/m3 for high-volume air samples, and 0.01-0.1 microgram/L for one-liter water samples. Applications were made to determination of pesticides in fogwater and air samples.

Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

Energy Technology Data Exchange (ETDEWEB)

Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W. [BgVV - Federal Inst. for Health Protection of Consumers and Veterinary Medicine, Berlin (Germany)

1996-12-31

The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author).

Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

International Nuclear Information System (INIS)

Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W.

1996-01-01

The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author)

Chromatographic and spectroscopic analysis of heavy crude oil mixtures with emphasis in nuclear magnetic resonance spectroscopy: A review

International Nuclear Information System (INIS)

Silva, Sandra L.; Silva, Artur M.S.; Ribeiro, Jorge C.; Martins, Fernando G.; Da Silva, Francisco A.; Silva, Carlos M.

2011-01-01

Graphical abstract: The chromatographic and spectroscopic techniques used to characterize heavy crude oils, although more focused in the nuclear magnetic resonance spectroscopy as the technique of choice, due to its capability to provide great information on the chemical nature of individual types of proton and carbon atoms in different and complex mixtures of crude oils are described. This review is based on 65 references and describes in a critical and interpretative ways the advantages of the NMR spectroscopy as a main technique to be used in crude oil refining industries that want to characterize crude oil fractions and the obtained refined products. Highlights: ► Chromatogrfaphic and spectroscopic techniques used to characterize heavy crude oils have been reviewed. ► This review describes in a critical and interpretative ways the advantages of the NMR spectroscopy as a main technique to be used in crude oil refining industries. ► The progress in the interpretation of the NMR spectra and of different multivariate data analyses and their potential in the identification and characterization of hydrocarbons and their physical and chemical properties have also been reviewed. - Abstract: The state of the art in the characterization of heavy crude oil mixtures is presented. This characterization can be done by different techniques, such as gas chromatography (GC), high performance liquid chromatography (HPLC), thin layer chromatography (TLC), infrared spectroscopy (IR), Raman spectroscopy, nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry (MS). Nuclear magnetic resonance spectroscopy is the technique of choice due to its capability to provide information on the chemical nature of individual types of hydrogen and carbon atoms in different and complex mixtures of crude oils. The progress made in the interpretation of the NMR spectra with the development of new NMR techniques and different multivariate data analyses could give relevant

Method for chromatographically recovering scandium and yttrium

International Nuclear Information System (INIS)

Snyder, T.S.; Stoltz, R.A.

1991-01-01

This paper describes a method for chromatographically recovering scandium and yttrium from the residue of a sand chlorinator. It comprises: providing a residue from a sand chlorinator, the residue containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; digesting the residue with an acid to produce an aqueous liquid containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; feeding the metal containing liquid through a cation exchanger; eluding the cation exchanger with an acid eluant to to produce: a first eluate containing at least half of the total weight of the calcium and sodium in the feed liquid; a second eluate containing at least half of the total weight of the one or more radioactive metals in the feed liquid; a third eluate containing at least half of the yttrium in the feed liquid, and a fourth eluate containing at least half of the weight of the scandium in the feed liquid

Investigating the Effect of Column Geometry on Separation Efficiency using 3D Printed Liquid Chromatographic Columns Containing Polymer Monolithic Phases.

Science.gov (United States)

Gupta, Vipul; Beirne, Stephen; Nesterenko, Pavel N; Paull, Brett

2018-01-16

Effect of column geometry on the liquid chromatographic separations using 3D printed liquid chromatographic columns with in-column polymerized monoliths has been studied. Three different liquid chromatographic columns were designed and 3D printed in titanium as 2D serpentine, 3D spiral, and 3D serpentine columns, of equal length and i.d. Successful in-column thermal polymerization of mechanically stable poly(BuMA-co-EDMA) monoliths was achieved within each design without any significant structural differences between phases. Van Deemter plots indicated higher efficiencies for the 3D serpentine chromatographic columns with higher aspect ratio turns at higher linear velocities and smaller analysis times as compared to their counterpart columns with lower aspect ratio turns. Computational fluid dynamic simulations of a basic monolithic structure indicated 44%, 90%, 100%, and 118% higher flow through narrow channels in the curved monolithic configuration as compared to the straight monolithic configuration at linear velocities of 1, 2.5, 5, and 10 mm s -1 , respectively. Isocratic RPLC separations with the 3D serpentine column resulted in an average 23% and 245% (8 solutes) increase in the number of theoretical plates as compared to the 3D spiral and 2D serpentine columns, respectively. Gradient RPLC separations with the 3D serpentine column resulted in an average 15% and 82% (8 solutes) increase in the peak capacity as compared to the 3D spiral and 2D serpentine columns, respectively. Use of the 3D serpentine column at a higher flow rate, as compared to the 3D spiral column, provided a 58% reduction in the analysis time and 74% increase in the peak capacity for the isocratic separations of the small molecules and the gradient separations of proteins, respectively.

Liquid chromatographic determination of aniline and derivatives in environmental waters at nanogram per litre levels using fluorescamine pre-column derivatization

Energy Technology Data Exchange (ETDEWEB)

Djozan, D. [Univ. of Tabriz (Iran, Islamic Republic of). Dept. of Analytical Chemistry; Faraj-Zadeh, M.A. [Univ. of Tabriz (Iran, Islamic Republic of). Dept. of Analytical Chemistry

1995-11-01

Fluorescamine (fluram) has been used as a fluorogenic compound for pre-column derivatization of aniline and some derivatives. Anilines were derivatized with fluram in citrate buffer media (pH 5.5) to form pyrrolinones. The highly fluorescence pyrrolinones were isolated and pre-concentrated by solid phase extraction. A reversed phase, Spherisorb RP-8 column and tetrahydrofuran: Water:formic acid (42:56:2) mobile phase was used for separation. Detection method was by a sensitive fluorimetric method and quantitation was at 395 and 495 nm. The various parameters such as reaction conditions between anilines and fluram, solid phase extraction and chromatographic separation were optimized. Calibrations were linear over the range considered with excellent correlation coefficients (r>0.999). Relative standard deviations are less than 2.5% and detection limits for aniline, p-toluidine, 4-chloroaniline and 4-bromoaniline were 6, 30, 6 and 8 ng L{sup -1}, respectively. This method has been used successfully for the determination of anilines in environmental waters. (orig.)

Characterizing the selectivity of stationary phases and organic modifiers in reversed-phase high-performance liquid chromatographic systems by a general solvation equation using gradient elution.

Science.gov (United States)

Du, C M; Valko, K; Bevan, C; Reynolds, D; Abraham, M H

2000-11-01

Retention data for a set of 69 compounds using rapid gradient elution are obtained on a wide range of reversed-phase stationary phases and organic modifiers. The chromatographic stationary phases studied are Inertsil (IN)-ODS, pentafluorophenyl, fluoro-octyl, n-propylcyano, Polymer (PLRP-S 100), and hexylphenyl. The organic solvent modifiers are 2,2,2-trifluoroethanol (TFE); 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP); isopropanol; methanol (MeOH); acetonitrile (AcN); tetrahydrofuran; 1,4-dioxane; N,N-dimethylformamide; and mixed solvents of dimethylsulfoxide (DMSO) with AcN and DMSO with MeOH (1:1). A total of 25 chromatographic systems are analyzed using a solvation equation. In general, most of the systems give reasonable statistics. The selectivity of the reversed phase-high-performance liquid chromatographic (HPLC) systems with respect to the solute's dipolarity-polarity, hydrogen-bond acidity, and basicity are reflected in correspondingly large coefficients in the solvation equation. We wanted to find the most orthogonal HPLC systems, showing the highest possible selectivity difference in order to derive molecular descriptors using the gradient retention times of a compound. We selected eight chromatographic systems that have a large range of coefficients of interest (s, a, and b) similar to those found in water-solvent partitions used previously to derive molecular descriptors. The systems selected are IN-ODS phases with AcN, MeOH, TFE, and HFIP as mobile phase, PLRP-S 100 phase with AcN, propylcyano phase with AcN and MeOH, and fluorooctyl phase with TFE. Using the retention data obtained for a compound in the selected chromatographic systems, we can estimate the molecular descriptors with the faster and simpler gradient elution method.

Analysis and Comparison of the Antioxidant Component of Portulaca Oleracea Leaves Obtained by Different Solid-Liquid Extraction Techniques

Science.gov (United States)

Conte, Esterina

2017-01-01

Portulaca oleracea is a wild plant pest of orchards and gardens, but is also an edible vegetable rich in beneficial nutrients. It possesses many antioxidant properties due to the high content of vitamins, minerals, omega-3 essential fatty acids and other healthful compounds; therefore, the intake of purslane and/or its bioactive compounds could help to improve the health and function of the whole human organism. Accordingly, in this work it was analyzed and compared to the extractive capacity of the antioxidant component of purslane leaves obtained by solid-liquid extraction techniques such as: hot-maceration, maceration with ultrasound, rapid solid-liquid dynamic extraction using the Naviglio extractor, and a combination of two techniques (mix extraction). The chromatographic analysis by High Performance Liquid Chromatography (HPLC) of the methanolic extract of dried purslane leaves allowed the identification of various polyphenolic compounds for comparison with the standards. In addition, the properties of the different extracts were calculated on dry matter and the antioxidant properties of the total polyphenol components analyzed by the DPPH (2,2-diphenyl-1-picrylhydrazyl) assay. The results showed that mix extraction was the most efficient compared to other techniques. In fact, it obtained a quantity of polyphenols amounting to 237.8 mg Gallic Acid Equivalents (GAE)/100 g of fresh weight, while in other techniques, the range varied from 60–160 mg GAE/100 g fresh weight. In addition, a qualitative analysis by Liquid Chromatography-Tandem Mass Spectrometry (LC/MS/MS) of the phenolic compounds present in the purslane leaves examined was carried out. The compounds were identified by comparison of their molecular weight, fragmentation pattern and retention time with those of standards, using the “Multiple Reaction Monitoring” mode (MRM). Therefore, this study allowed the re-evaluation of a little-known plant that possesses as its beneficial properties, a

Liquid chromatographic-tandem mass spectrometric method for the simultaneous determination of alkylphenols polyethoxylates, alkylphenoxy carboxylates and alkylphenols in wastewater and surface-water.

Science.gov (United States)

Ciofi, L; Ancillotti, C; Chiuminatto, U; Fibbi, D; Checchini, L; Orlandini, S; Del Bubba, M

2014-10-03

Four different pellicular stationary phases (i.e. octadecylsilane, octasilane, Phenyl-Hexyl and pentafluorophenyl) were investigated for the chromatographic resolution of alkylphenols (APs), alkylphenols polyethoxylates (APnEOs) and alkylphenoxy carboxylates (APECs) using mixtures of water and organic solvents (i.e. methanol, acetonitrile and tetrahydrofuran) as eluents, in order to obtain their determination by a single LC-MS/MS run. In fact, alkylphenols and alkylphenoxy carboxylates must be analysed in negative ion mode, whereas alkylphenols polyethoxylates undergo ionisation only in positive ion mode, and therefore, two distinct LC-MS/MS analysis are commonly adopted. The best resolution among the aforementioned target analytes was achieved on the pentafluorophenyl column, eluting with an acidified water-acetonitrile-tetrahydrofuran mixture and using the post column addition of an ammonia solution in methanol for the detection of positively ionisable compounds. Under these optimized chromatographic conditions the investigated compounds were determined via a single chromatographic run, with only one polarity switch, in 15min, achieving the following instrumental detection limits: 600pg for AP1EOs, 0.8-14pg for AP2EOs, 10.4-150pg for APs and 4.4-4.8pg for APECs. The chromatographic method was coupled with solid-phase extraction and clean-up procedures and successfully applied to the analysis of wastewater and surface water samples, highlighting mean concentration ranging from 6ng/L for 4-t-OP1EC to 1434ng/L for 4-NP1121EC, depending on the sample analysed. Copyright © 2014 Elsevier B.V. All rights reserved.

Importance of MS selectivity and chromatographic separation in LC-MS/MS-based methods when investigating pharmaceutical metabolites in water. Dipyrone as a case of study.

Science.gov (United States)

Ibáñez, M; Gracia-Lor, E; Sancho, J V; Hernández, F

2012-08-01

Pharmaceuticals are emerging contaminants of increasing concern because of their presence in the aquatic environment and potential to reach drinking-water sources. After human and/or veterinary consumption, pharmaceuticals can be excreted in unchanged form, as the parent compound, and/or as free or conjugated metabolites. Determination of most pharmaceuticals and metabolites in the environment is commonly made by liquid chromatography (LC) coupled to mass spectrometry (MS). LC coupled to tandem MS is the technique of choice nowadays in this field. The acquisition of two selected reaction monitoring (SRM) transitions together with the retention time is the most widely accepted criterion for a safe quantification and confirmation assay. However, scarce attention is normally paid to the selectivity of the selected transitions as well as to the chromatographic separation. In this work, the importance of full spectrum acquisition high-resolution MS data using a hybrid quadrupole time-of-flight analyser and/or a suitable chromatographic separation (to reduce the possibility of co-eluting interferences) is highlighted when investigating pharmaceutical metabolites that share common fragment ions. For this purpose, the analytical challenge associated to the determination of metabolites of the widely used analgesic dipyrone (also known as metamizol) in urban wastewater is discussed. Examples are given on the possibilities of reporting false positives of dypirone metabolites by LC-MS/MS under SRM mode due to a wrong assignment of identity of the compounds detected. Copyright © 2012 John Wiley & Sons, Ltd.

Chromatographic evaluation and antimicrobial activity of Neem (Azadirachta indica A. Juss., Meliaceae leaves hydroalcoholic extracts

Directory of Open Access Journals (Sweden)

Priscila D. Alves

Full Text Available Neem (Azadirachta indica is an Indian tree well known for its several pharmacological activities, including antimicrobial activity. More than 300 composites have already been isolated and azadirachtin (AZA is its main active component. In the present work, Neem leaves hydroalcoholic extracts were prepared by percolation in 96% ethanol different concentrations (50%, 60%, 70%, 80% and 90% (v/v. The presence of AZA was tested by TLC by eluting the extracts and a standard solution of AZA through a chromatographic plate developed with anisaldehyde/sulfuric acid solution followed by heating. By HPLC, extracts elution took place on a C18 column, water:acetonitrile (60:40 as mobile phase, 1.0 mL/min flow rate and detection at λ217 nm. The extracts did not display AZA spots or peaks, however, they were tested against Gram-positive and Gram-negative bacteria, yeasts and a mold fungus. The extracts were tested in different increasing concentrations, in order to detect a dose-dependent relationship of the activity. Despite the absence of AZA, the 70% and 80% (v/v ethanol extracts showed activity against Staphylococcus aureus. However, this activity was not dose-dependent according to Tukey's test (q0,05;3;7.

Fundulus heteroclitus gonadotropins.5: Small scale chromatographic fractionation of pituitary extracts into components with different steroidogenic activities using homologous bioassays

Directory of Open Access Journals (Sweden)

Petrino Teresa R

2004-03-01

Full Text Available Abstract Fractionation and characterization of gonadotropins (GtH from Fundulus heteroclitus pituitary extracts were carried out using a biocompatible liquid chromatographic procedure (Pharmacia FPLC system. Chromatographic fractions were monitored for gonadotropic activities (induction of oocyte maturation and steroid production using homologous follicle bioassays in vitro. Size-exclusion chromatography eluted gonadotropic activity in one major protein peak (Mr ~ 30,000. Anion-exchange and hydrophobic-interaction chromatography (HIC yielded two distinct peaks of 17beta-estradiol (E2- and 17alpha-hydroxy,20beta-dihydroprogesterone (DHP-promoting activity with associated oocyte maturation. Two-dimensional chromatography (chromatofocusing followed by HIC resolved pituitary extracts into two active fractions; both induced E2 synthesis, but one was relatively poor in eliciting DHP and testosterone production. Thus, using homologous bioassays, at least two quantitatively different gonadotropic (steroidogenic activities: an E2-promoting gonadotropin (GtH I-like and a DHP-promoting gonadotropin (GtH II-like, which has a lower isoelectric point but greater hydrophobicity than the former, can be distinguished from F. heteroclitus pituitaries by a variety of chromatographic procedures. This study complements previous biochemical and molecular data in F. heteroclitus and substantiates the duality of GtH function in a multiple-spawning teleost.

Laparoscopic colorectal surgery in learning curve: Role of implementation of a standardized technique and recovery protocol. A cohort study

Directory of Open Access Journals (Sweden)

Gaetano Luglio

2015-06-01

Conclusion: Proper laparoscopic colorectal surgery is safe and leads to excellent results in terms of recovery and short term outcomes, even in a learning curve setting. Key factors for better outcomes and shortening the learning curve seem to be the adoption of a standardized technique and training model along with the strict supervision of an expert colorectal surgeon.

Direct coupling of a liquid chromatograph to a continuous flow hydrogen nuclear magnetic resonance detector for analysis of petroleum and synthetic fuels

International Nuclear Information System (INIS)

Haw, J.F.; Glass, T.E.; Hausler, D.W.; Motell, E.; Dorn, H.C.

1980-01-01

Initial results obtained for a flow 1 H nuclear magnetic resonance (NMR) detector directly coupled to a liquid chromatography unit are described. Results achieved for a model mixture and several jet fuel samples are discussed. Chromatographic separation of alkanes, alkylbenzenes, and substituted naphthalenes present in the jet fuel samples are easily identified with the 1 H NMR detector. Results with our present flow 1 H NMR insert indicate that 5-Hz linewidths are readily obtainable for typical chromatographic flow rates. The limitations and advantages of this liquid chromatography detector are compared with more commonly employed detectors (e.g., refractive index detectors). 11 figures

Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

Science.gov (United States)

Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

2014-10-03

Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

Chromatographic separation of radioactive noble gases from xenon

Science.gov (United States)

Akerib, D. S.; Araújo, H. M.; Bai, X.; Bailey, A. J.; Balajthy, J.; Beltrame, P.; Bernard, E. P.; Bernstein, A.; Biesiadzinski, T. P.; Boulton, E. M.; Bramante, R.; Cahn, S. B.; Carmona-Benitez, M. C.; Chan, C.; Chiller, A. A.; Chiller, C.; Coffey, T.; Currie, A.; Cutter, J. E.; Davison, T. J. R.; Dobi, A.; Dobson, J. E. Y.; Druszkiewicz, E.; Edwards, B. N.; Faham, C. H.; Fiorucci, S.; Gaitskell, R. J.; Gehman, V. M.; Ghag, C.; Gibson, K. R.; Gilchriese, M. G. D.; Hall, C. R.; Hanhardt, M.; Haselschwardt, S. J.; Hertel, S. A.; Hogan, D. P.; Horn, M.; Huang, D. Q.; Ignarra, C. M.; Ihm, M.; Jacobsen, R. G.; Ji, W.; Kamdin, K.; Kazkaz, K.; Khaitan, D.; Knoche, R.; Larsen, N. A.; Lee, C.; Lenardo, B. G.; Lesko, K. T.; Lindote, A.; Lopes, M. I.; Manalaysay, A.; Mannino, R. L.; Marzioni, M. F.; McKinsey, D. N.; Mei, D.-M.; Mock, J.; Moongweluwan, M.; Morad, J. A.; Murphy, A. St. J.; Nehrkorn, C.; Nelson, H. N.; Neves, F.; O'Sullivan, K.; Oliver-Mallory, K. C.; Palladino, K. J.; Pease, E. K.; Pech, K.; Phelps, P.; Reichhart, L.; Rhyne, C.; Shaw, S.; Shutt, T. A.; Silva, C.; Solovov, V. N.; Sorensen, P.; Stephenson, S.; Sumner, T. J.; Szydagis, M.; Taylor, D. J.; Taylor, W.; Tennyson, B. P.; Terman, P. A.; Tiedt, D. R.; To, W. H.; Tripathi, M.; Tvrznikova, L.; Uvarov, S.; Verbus, J. R.; Webb, R. C.; White, J. T.; Whitis, T. J.; Witherell, M. S.; Wolfs, F. L. H.; Yazdani, K.; Young, S. K.; Zhang, C.

2018-01-01

The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes 85Kr and 39Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search experiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

New materials for sample preparation techniques in bioanalysis.

Science.gov (United States)

Nazario, Carlos Eduardo Domingues; Fumes, Bruno Henrique; da Silva, Meire Ribeiro; Lanças, Fernando Mauro

2017-02-01

The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche. Copyright © 2016 Elsevier B.V. All rights reserved.

Technical Note: Precise quantitative measurements of total dissolved inorganic carbon from small amounts of seawater using a gas chromatographic system

Directory of Open Access Journals (Sweden)

T. Hansen

2013-10-01

Full Text Available Total dissolved inorganic carbon (CT is one of the most frequently measured parameters used to calculate the partial pressure of carbon dioxide in seawater. Its determination has become increasingly important because of the rising interest in the biological effects of ocean acidification. Coulometric and infrared detection methods are currently favored in order to precisely quantify CT. These methods however are not sufficiently validated for CT measurements of biological experiments manipulating seawater carbonate chemistry with an extended CT measurement range (~1250–2400 μmol kg–1 compared to natural open ocean seawater (~1950–2200 μmol kg−1. The requirement of total sample amounts between 0.1–1 L seawater in the coulometric- and infrared detection methods potentially exclude their use for experiments working with much smaller volumes. Additionally, precise CT analytics become difficult with high amounts of biomass (e.g., phytoplankton cultures or even impossible in the presence of planktonic calcifiers without sample pre-filtration. Filtration however, can alter CT concentration through gas exchange induced by high pressure. Addressing these problems, we present precise quantification of CT using a small, basic and inexpensive gas chromatograph as a CT analyzer. Our technique is able to provide a repeatability of ±3.1 μmol kg−1, given by the pooled standard deviation over a CT range typically applied in acidification experiments. 200 μL of sample is required to perform the actual CT measurement. The total sample amount needed is 12 mL. Moreover, we show that sample filtration is applicable with only minor alteration of the CT. The method is simple, reliable and with low cumulative material costs. Hence, it is potentially attractive for all researchers experimentally manipulating the seawater carbonate system.

Abnormal tyrosine and phenylalanine metabolism in patients with tyrosyluria and phenylketonuria; gas-liquid chromatographic analysis of urinary metabolites

NARCIS (Netherlands)

Wadman, S.K.; Heiden, C. van der; Ketting, D.; Sprang, F.J. van

Gas-liquid chromatographic methods have been developed for the analysis of: urinary phenylalanine metabolites (I) in patients with phenylketonuria, tyrosine metabolites (II) in patients with a disturbed tyrosine metabolism at the level of p-hydroxyphenylpyruvate hydroxylase, and homogentisic acid in

Gas chromatographic simulated distillation-mass spectrometry for the determination of the boiling point distributions of crude oils

Science.gov (United States)

Roussis; Fitzgerald

2000-04-01

The coupling of gas chromatographic simulated distillation with mass spectrometry for the determination of the distillation profiles of crude oils is reported. The method provides the boiling point distributions of both weight and volume percent amounts. The weight percent distribution is obtained from the measured total ion current signal. The total ion current signal is converted to weight percent amount by calibration with a reference crude oil of a known distillation profile. Knowledge of the chemical composition of the crude oil across the boiling range permits the determination of the volume percent distribution. The long-term repeatability is equivalent to or better than the short-term repeatability of the currently available American Society for Testing and Materials (ASTM) gas chromatographic method for simulated distillation. Results obtained by the mass spectrometric method are in very good agreement with results obtained by conventional methods of physical distillation. The compositional information supplied by the method can be used to extensively characterize crude oils.

Liquid chromatographic determination of oxytetracycline in edible fish fillets from six species of fish

Science.gov (United States)

Meinertz, J.R.; Stehly, G.R.; Gingerich, W.H.

1998-01-01

The approved use of oxytetracycline (OTC) in U.S. Aquaculture is limited to specific diseases in salmonids and channel catfish. OTC may also be effective in controlling diseases in other fish species important to public aquaculture, but before approved use of OTC can be augmented, an analytical method for determining OTC in fillet tissue from multiple species of fish will be required to support residue depletion studies. The objective of this study was to develop and validate a liquid chromatographic (LC) method that is accurate, precise, and sensitive for OTC in edible fillets from multiple species of fish. Homogenized fillet tissues from walleye, Atlantic salmon, striped bass, white sturgeon, rainbow trout, and channel catfish were fortified with OTC at nominal concentrations of 10, 20, 100, 1000, and 5000 ng/g. In tissues fortified with OTC at 100, 1000, and 5000 ng/g, mean recoveries ranged from 83 to 90%, and relative standard deviations (RSDs) ranged from 0.9 to 5.8%. In all other tissues, mean recoveries ranged from 59 to 98%, and RSDs ranged from 3.3 to 20%. Method quantitation limits ranged from 6 to 22 ng/g for the 6 species. The LC parameters produced easily integratable OTC peaks without coelution of endogenous compounds. The method is accurate, precise, and sensitive for OTC in fillet tissue from 6 species of fish from 5 phylogenetically diverse groups.

Ion chromatographic determination of fluoride and chloride in UO2 using microbore anion exchange columns

International Nuclear Information System (INIS)

Kelkar, Anoop; Meena, D.L.; Das, D.K.; Behere, P.G.; Mohd Afzal

2015-01-01

Chemical characterization of nuclear fuels is required to ensure that nuclear fuel meets the technical specifications of the fuel. Trace non- metallic impurities like Cl and F is important as they affect clad corrosion. Their effect is more severe in presence of moisture. Chlorine and Fluorine is routinely analysed by ion selective electrode or conventional ion chromatography after pyrohydrolyzing the sample in moist O 2 atmosphere at 950°. Both the technique generates large quantity of liquid waste. Generally 1 ml/min flow rate required for the separation of F - and Cl - in conventional ion-chromatographic separation of F - and Cl - on 4.6- 4.0 mm id analytical column. The waste produced per sample injection is ∼ 30-40 ml with suppressed conductivity detection in ion chromatography. There is a need to reduce this analytical waste in analyzing the radioactive samples for the determination of F - and Cl - . Waste generation could be effectively reduced by using microbore anion exchange analytical column. Present paper describe the use of Metrosep A Supp 16 - 100/2.0 column with Na 2 CO 3 +NaOH mobile phase for the determination of F - and Cl - in UO 2 samples using suppressed conductivity detection

Assessment of chromium biostabilization in contaminated soils using standard leaching and sequential extraction techniques

International Nuclear Information System (INIS)

Papassiopi, Nymphodora; Kontoyianni, Athina; Vaxevanidou, Katerina; Xenidis, Anthimos

2009-01-01

The iron reducing microorganism Desulfuromonas palmitatis was evaluated as potential biostabilization agent for the remediation of chromate contaminated soils. D. palmitatis were used for the treatment of soil samples artificially contaminated with Cr(VI) at two levels, i.e. 200 and 500 mg kg -1 . The efficiency of the treatment was evaluated by applying several standard extraction techniques on the soil samples before and after treatment, such as the EN12457 standard leaching test, the US EPA 3060A alkaline digestion method and the BCR sequential extraction procedure. The water soluble chromium as evaluated with the EN leaching test, was found to decrease after the biostabilization treatment from 13 to less than 0.5 mg kg -1 and from 120 to 5.6 mg kg -1 for the soil samples contaminated with 200 and 500 mg Cr(VI) per kg soil respectively. The BCR sequential extraction scheme, although not providing accurate estimates about the initial chromium speciation in contaminated soils, proved to be a useful tool for monitoring the relative changes in element partitioning, as a consequence of the stabilization treatment. After bioreduction, the percentage of chromium retained in the two least soluble BCR fractions, i.e. the 'oxidizable' and 'residual' fractions, increased from 54 and 73% to more than 96% in both soils

Development and validation of a HPLC method for standardization of herbal and commercial extracts of Myrcia uniflora

Directory of Open Access Journals (Sweden)

Andrea N. de L. Batista

2011-06-01

Full Text Available Myrcia uniflora Barb. Rodr., Myrtaceae, popularly known as "pedra-hume-caá" in Brazil, is sold as dry extracts in capsules or as tinctures for the treatment of diabetes mellitus. Previous phytochemical studies on this species described the occurrence of the flavonoids mearnsitrin and myricitrin. In the present study, the chromatographic profiles of M. uniflora leaves and commercial extracts were determined using HPLC-PAD. Myricitrin was used as an external standard in the development and validation of the HPLC method. The proposed method is simple, rapid and reliable and can be successfully applied in industry for standardization of herbs and phytomedicines commercialised in Brazil as "pedra-hume-caá".

Development and validation of a HPLC method for standardization of herbal and commercial extracts of Myrcia uniflora

Directory of Open Access Journals (Sweden)

Andrea N. de L. Batista

2011-04-01

Full Text Available Myrcia uniflora Barb. Rodr., Myrtaceae, popularly known as "pedra-hume-caá" in Brazil, is sold as dry extracts in capsules or as tinctures for the treatment of diabetes mellitus. Previous phytochemical studies on this species described the occurrence of the flavonoids mearnsitrin and myricitrin. In the present study, the chromatographic profiles of M. uniflora leaves and commercial extracts were determined using HPLC-PAD. Myricitrin was used as an external standard in the development and validation of the HPLC method. The proposed method is simple, rapid and reliable and can be successfully applied in industry for standardization of herbs and phytomedicines commercialised in Brazil as "pedra-hume-caá".

37Ar monitoring techniques and on-site inspection system

International Nuclear Information System (INIS)

Duan Rongliang; Chen Yinliang; Li Wei; Wang Hongxia; Hao Fanhua

2001-01-01

37 Ar is separated, purified and extracted from air sample with a low temperature gas-solid chromatographic purifying method, prepared into a radioactive measurement source and its radioactivity is measured with a proportional counter. Based on the monitoring result, a judgement can be made if an nuclear explosion event has happened recently in a spectabilis area. A series of element techniques that are associated the monitoring of the trace element 37 Ar have been investigated and developed. Those techniques include leaked gas sampling, 37 Ar separation and purification, 37 Ar radioactivity measurement and the on-site inspection of 37 Ar. An advanced 37 Ar monitoring method has been developed, with which 200 liters of air can be treated in 2 hours with sensitivity of 0.01 Bq/L for 37 Ar radioactivity measurement. A practical 37 Ar On-site Inspection system has been developed. This research work may provide technical and equipment support for the verification protection, verification supervision and CTBT verification