Investigation of Some Potent Medicinal Plants of N.E.INDIA with Respect to Thermophysical, Chromatographic and Crystallographic Properties

Science.gov (United States)

Bora, M. N.; Kalita, Mahendra

2010-06-01

North East India is readily available of various kinds of medicinal plants. A lot of studies on thermophysical properties of plant leaves, fluids, stems and roots had already been made[3,4,8]. In the present studies of thermophysical properties, chromatographic and crystallographic properties of specific medicinal plant leaves (Azadirechta indica)A, (Vinca rosea)B, (Clerodrendrum colebrookianum)C, (Osimum sanctum)D and fruits (Chisocheton paniculatus) E, and (Cudrania javanensis) F have been made plant based drugs for curing for different chronic diseases. The thermophysical properties of these leaves and fruits have been studies with XRD, XRF, TG, DTG, DTA, and DSC thermograms. From weight loss(%), time and temperature variations, the Activation Energies of these medicinal plant samples have been computed. The thermal stability is found more for the fruits samples than that of the leave samples. Thermal behaviours of all six samples have shown hygroscopic behaviour. The results TG, DTG and DTA thermograms confirmed that all samples show similar dehydration and decomposition reactions and hydrophilic nature. Both chromatographic techniques thin layer (TLC) and Column chromatography have been used for separation of components of the mixtures of samples. From these methods of the fruit sample E a pure crystalline white solids have been identified and confirm them as (MK 01) α-isomer. Our interest to study the molecular and crystal structure of the sample E. The single crystal of (MK 01) is found to be orthorhombic cell with lattice parameters a = 10ṡ699(3)Å b = 15ṡ5100(4)Å c = 16ṡ626(4)Å α = 90° β = 90° γ = 90° with space group P212121 Again from fruit sample F a light yellow solid is isolated and on crystallization give crystalline solid MN-01 and MN-02 and it is confirmed that these two compounds are unsaturated isoflavonoids. The single crystal of MN-01 has been found monoclinic with lattice parameters a = 6.2374(11)Å, b = 8.4243(11)Å, c = 21

Antioxidant and Antiangiogenic Properties, and Gas Chromatographic-Time of Flight Analysis of Sonchus arvensis Leaves Extracts

International Nuclear Information System (INIS)

Itam, A.; Shah, A. M.; Majid, A.; Ismail, Z.

2015-01-01

Sonchus arvensis L. (Asteraceae) is one of the medicinal herbs used in traditional medicines, in which the leaf extract was used as a diuretic, lithotriptic and antiurolithiasis agent. The leaves of S. arvensis reported contain several compounds, including a variety of flavonoids, terpenoids and sterol, even this plant also contain silica and potassium. Flavonoids are secondary metabolite compound which have ability as antioxidant. In this study, the aims are to determine of antioxidants and antiangiogenic properties, and phytoconstituents quantitative of aqueous and methanol extracts of S. arvensis leaves. The antioxidant properties were studied using 1,1-Diphenyl-2-picrylhydrazyl (DPPH) free radical, xanthine oxidase and beta-carotene-linoleate models system. Furthermore, the antiangiogenic property was evaluated using ex vivo rat aorta ring assay. Quantitative determination of extracts phytoconstituents were carried out by using Gas Chromatographic-Time of Flight (GC-TOF) mass spectrophotometric methods. The results showed that the aqueous and methanol extracts have ability as antioxidant which is antioxidant activities of aqueous extracts on DPPH radical and inhibition of xanthine oxidase activity are higher than that of methanol extracts. Meanwhile antioxidant activity using beta-carotene-linoleate model system of S. arvensis aqueous extract is lower than that of methanol extracts. Nevertheless, the differences of these antioxidant activities are not significant. Antiangiogenic property of aqueous extract is also higher than that of methanol extract which is measured at 100 meu g mL/sup -1/ of extracts. This indicates that there is correlation between antioxidant activity and antiangigenic property, exhibiting that this plant possesses the potential to prevent or cure the diseases that related to angiogenesis such as cancer. (author)

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

The impact of functional jaw orthopedics in subjects with unfavorable Class II skeletal patterns.

Science.gov (United States)

Baccetti, Tiziano; McNamara, James A

2010-01-01

To evaluate the outcomes of functional jaw orthopedics (FJO) followed by fixed appliances in Class II patients showing cephalometric signs predictive of unfavorable responsiveness to orthopedic treatment. A total of 48 treated subjects (20 males, 28 females) with unfavorable Class II malocclusions were treated with FJO at the adolescent growth spurt, followed by fixed appliances. Treatment outcomes were compared with the growth changes in a matched control group of untreated subjects with "unfavorable" Class II malocclusions. A significant prevalence rate of successful outcome was recorded within the treated group (64.5%). When compared with the untreated controls, both the overall treated group and the successful treated subgroup revealed a significant reduction in maxillary growth and sagittal position, along with a significant enhancement in mandibular length, sagittal advancement of the mandible, and significant improvements in the maxillo-mandibular relationships. Both overjet and molar relation showed significant favorable changes in the treated group. FJO at the pubertal spurt followed by fixed appliances is a viable therapeutical option in patients with "unfavorable" Class II malocclusions, although skeletal changes are of minor entity. Copyright © 2010 Società Italiana di Ortodonzia SIDO. Published by Elsevier Srl. All rights reserved.

Predictive factors of unfavorable prostate cancer in patients who underwent prostatectomy but eligible for active surveillance

Directory of Open Access Journals (Sweden)

Seol Ho Choo

2014-06-01

Conclusions: A significant proportion of patients who were candidates for active surveillance had unfavorable prostate cancer. Age, PSA density, and two positive cores were independent significant predictive factors for unfavorable prostate cancer. These factors should be considered when performing active surveillance.

Treatment With JAK Inhibitors in Myelofibrosis Patients Nullifies the Prognostic Impact of Unfavorable Cytogenetics.

Science.gov (United States)

Ma, Vincent T; Boonstra, Philip S; Menghrajani, Kamal; Perkins, Cecelia; Gowin, Krisstina L; Mesa, Ruben A; Gotlib, Jason R; Talpaz, Moshe

2018-05-01

In the era before Janus kinase (JAK) inhibitors, cytogenetic information was used to predict survival in myelofibrosis patients. However, the prognostic value of cytogenetics in the setting of JAK inhibitor therapy remains unknown. We performed a retrospective analysis of 180 patients with bone marrow biopsy-proven myelofibrosis from 3 US academic medical centers. We fit Cox proportional hazards models for overall survival and transformation-free survival on the bases of 3 factors: JAK inhibitor therapy as a time-dependent covariate, dichotomized cytogenetic status (favorable vs. unfavorable), and statistical interaction between the two. The median follow-up time was 37.1 months. Among patients treated with best available therapy, unfavorable cytogenetic status was associated with decreased survival (hazard ratio = 2.31; P = .025). At initiation of JAK inhibitor therapy, unfavorable cytogenetics was (nonsignificantly) associated with increased survival compared to favorable cytogenetics (hazard ratio = 0.292; P = .172). The ratio of hazard ratios was 0.126 (P = .034). These findings were similar after adjusting for standard clinical prognostic factors as well as when measured against transformation-free survival. The initiation of JAK inhibitor therapy appears to change the association between cytogenetics and overall survival. There was little difference in survival between treatment types in patients with favorable cytogenetics. However, the use of JAK inhibitor therapy among patients with unfavorable cytogenetics was not associated with worse survival compared to favorable cytogenetics. Our analyses suggest that initiation of JAK inhibitor therapy nullifies the negative prognostic implication of unfavorable cytogenetics established in the pre-JAK inhibitor therapy era. Copyright © 2018 The Authors. Published by Elsevier Inc. All rights reserved.

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

Going All In: Unfavorable Sex Ratios Attenuate Choice Diversification.

Science.gov (United States)

Ackerman, Joshua M; Maner, Jon K; Carpenter, Stephanie M

2016-06-01

When faced with risky decisions, people typically choose to diversify their choices by allocating resources across a variety of options and thus avoid putting "all their eggs in one basket." The current research revealed that this tendency is reversed when people face an important cue to mating-related risk: skew in the operational sex ratio, or the ratio of men to women in the local environment. Counter to the typical strategy of choice diversification, findings from four studies demonstrated that the presence of romantically unfavorable sex ratios (those featuring more same-sex than opposite-sex individuals) led heterosexual people to diversify financial resources less and instead concentrate investment in high-risk/high-return options when making lottery, stock-pool, retirement-account, and research-funding decisions. These studies shed light on a key process by which people manage risks to mating success implied by unfavorable interpersonal environments. These choice patterns have important implications for mating behavior as well as other everyday forms of decision making. © The Author(s) 2016.

Optimization of the gas chromatographic separations

International Nuclear Information System (INIS)

Gasco Sanchez, L.

1973-01-01

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

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.

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.

Comparison of job stress and obesity in nurses with favorable and unfavorable work schedules.

Science.gov (United States)

Han, Kihye; Trinkoff, Alison M; Storr, Carla L; Geiger-Brown, Jeanne; Johnson, Karen L; Park, Sungae

2012-08-01

To compare obesity-related factors between female nurses with favorable work schedules (WSs) and unfavorable WSs. In a cross-sectional study, 1724 female nurses were stratified by WS (favorable vs unfavorable). For each schedule type, the odds of obesity were related to health behaviors, home demands, and job stress using logistic regression models. Among nurses with unfavorable WSs, healthy behaviors (exercise, sleep) were inversely associated with obesity, whereas for those with favorable WSs, obese nurses reported significantly more unhealthy behaviors (smoking, alcohol use; odds ratio [OR], 1.19; 95% confidence interval [CI], 1.02-1.38), more physical lifting of children/dependents (OR, 1.43; 95% CI, 1.06-1.93), having more nurse input into their jobs (OR, 1.21; 95% CI, 1.02-1.44), yet less boss support at work (OR, 0.83; 95% CI, 0.68-0.99). Considering impacts of WSs on obesity and potential obesity-related health outcomes, healthful scheduling should be provided to nurses.

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.)

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.

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...

Effects of chromatographic fractions of Euphorbia hirta on the rat ...

African Journals Online (AJOL)

The effects of the chromatographic fractions of Euphorbia hirta Linn on the serum biochemical parameters in rats were investigated. The ethanolic extract of this plant was subjected to chromatographic separation using the vacuum liquid chromatographic technique, a modified form of classical column chromatography.

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.

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

Compensation for unfavorable characteristics of irregular individual shift rotas.

Science.gov (United States)

Knauth, Peter; Jung, Detlev; Bopp, Winfried; Gauderer, Patric C; Gissel, Andreas

2006-01-01

Some employees of TV companies, such as those who produce remote TV programs, have to cope with very irregular rotas and many short-term schedule deviations. Many of these employees complain about the negative effects of such on their wellbeing and private life. Therefore, a working group of employers, council representatives, and researchers developed a so-called bonus system. Based on the criteria of the BESIAK system, the following list of criteria for the ergonomic assessment of irregular shift systems was developed: proportion of night hours worked between 22 : 00 and 01 : 00 h and between 06 : 00 and 07 : 00 h, proportion of night hours worked between 01 : 00 and 06 : 00 h, number of successive night shifts, number of successive working days, number of shifts longer than 9 h, proportion of phase advances, off hours on weekends, work hours between 17 : 00 and 23 : 00 h from Monday to Friday, number of working days with leisure time at remote places, and sudden deviations from the planned shift rota. Each individual rota was evaluated in retrospect. If pre-defined thresholds of criteria were surpassed, bonus points were added to the worker's account. In general, more bonus points add up to more free time. Only in particular cases was monetary compensation possible for some criteria. The bonus point system, which was implemented in the year 2002 for about 850 employees of the TV company, has the advantages of more transparency concerning the unfavorable characteristics of working-time arrangements, incentive for superiors to design "good" rosters that avoid the bonus point thresholds (to reduce costs), positive short-term effects on the employee social life, and expected positive long-term effects on the employee health. In general, the most promising approach to cope with the problems of shift workers in irregular and flexible shift systems seems to be to increase their influence on the arrangement of working times. If this is not possible, bonus point systems

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.

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

The effect of charged groups on hydrophilic monolithic stationary phases on their chromatographic properties.

Science.gov (United States)

Li, Haibin; Liu, Chusheng; Wang, Qiqin; Zhou, Haibo; Jiang, Zhengjin

2016-10-21

In order to investigate the effect of charged groups present in hydrophilic monolithic stationary phases on their chromatographic properties, three charged hydrophilic monomers, i.e. N,N-dimethyl-N-acryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPDA), [2-(acryloyloxy)ethyl]trimethylammonium chloride (AETA), and 3-sulfopropyl acrylate potassium salt (SPA) were co-polymerized with the crosslinker N,N'-methylenebisacrylamide (MBA), respectively. The physicochemical properties of the three resulting charged hydrophilic monolithic columns were evaluated using scanning electron microscopy, ζ-potential analysis and micro-HPLC. High column efficiency was obtained on the three monolithic columns at a linear velocity of 1mm/s using thiourea as test compound. Comparative characterization of the three charged HILIC phases was then carried out using a set of model compounds, including nucleobases, nucleosides, benzoic acid derivatives, phenols, β-blockers and small peptides. Depending on the combination of stationary phase/mobile phase/solute, both hydrophilic interaction and other potential secondary interactions, including electrostatic interaction, hydrogen-bonding interaction, molecular shape selectivity, could contribute to the over-all retention of the analytes. Because of the strong electrostatic interaction provided by the quaternary ammonium groups in the poly (AETA-co-MBA) monolith, this cationic HILIC monolith exhibited the strongest retention for benzoic acid derivatives and small peptides with distorted peak shapes and the weakest retention for basic β-blockers. The sulfonyl groups on the poly (SPA-co-MBA) hydrophilic monolith could provide strong electrostatic attraction and hydrogen bonding for positively charged analytes and hydrogen-donor/acceptor containing analytes, respectively. Therefore, basic drugs, nucleobases and nucleotides exhibited the strongest retention on this anionic monolith. Because of the weak but distinct cation exchange properties of

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.

Low-Dose Consolidation Radiation Therapy for Early Stage Unfavorable Hodgkin Lymphoma

Energy Technology Data Exchange (ETDEWEB)

Torok, Jordan A., E-mail: jordan.torok@dm.duke.edu [Department of Radiation Oncology, Duke University Medical Center, Durham, North Carolina (United States); Wu, Yuan [Department of Biostatistics and Bioinformatics, Duke University Medical Center, Durham, North Carolina (United States); Prosnitz, Leonard R.; Kim, Grace J. [Department of Radiation Oncology, Duke University Medical Center, Durham, North Carolina (United States); Beaven, Anne W.; Diehl, Louis F. [Division of Hematologic Malignancy and Cellular Therapy, Department of Medicine, Duke University Medical Center, Durham, North Carolina (United States); Kelsey, Chris R. [Department of Radiation Oncology, Duke University Medical Center, Durham, North Carolina (United States)

2015-05-01

Purpose: The German Hodgkin Study Group (GHSG) trial HD11 established 4 cycles of doxorubicin, bleomycin, vinblastine, and dacarbazine (ABVD) and 30 Gy of radiation therapy (RT) as a standard for early stage (I, II), unfavorable Hodgkin lymphoma (HL). Additional cycles of ABVD may allow for a reduction in RT dose and improved toxicity profile. Methods and Materials: Patients treated with combined modality therapy at the Duke Cancer Institute for early stage, unfavorable HL by GHSG criteria from 1994 to 2012 were included. Patients who did not undergo post-chemotherapy functional imaging (positron emission tomography or gallium imaging) or who failed to achieve a complete response were excluded. Clinical outcomes were estimated using the Kaplan-Meier method. Late effects were also evaluated. Results: A total of 90 patients met inclusion criteria for analysis. Median follow-up was 5 years. Chemotherapy consisted primarily of ABVD (88%) with a median number of 6 cycles. The median dose of consolidation RT was 23.4 Gy. Four patients had relapses, 2 of which were in-field. Ten-year progression-free survival (PFS) and overall survival (OS) were 93% (95% confidence interval [CI]: 0.82-0.97) and 98% (95% CI: 0.92-0.99), respectively. For the subset of patients (n=46) who received 5 to 6 cycles of chemotherapy and ≤24 Gy, the 10-year PFS and OS values were 88% (95% CI: 70%-96%) and 98% (95% CI: 85% - 99%), respectively. The most common late effect was hypothyroidism (20%) with no cardiac complications. Seven secondary malignancies were diagnosed, with only 1 arising within the RT field. Conclusions: Lower doses of RT may be sufficient when combined with more than 4 cycles of ABVD for early stage, unfavorable HL and may result in a more favorable toxicity profile than 4 cycles of ABVD and 30 Gy of RT.

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.

Unfavorable results in replantation

Directory of Open Access Journals (Sweden)

Abraham G Thomas

2013-01-01

Full Text Available Reattachment of amputated parts of the body (Replantation has become a reality since the first arm replant was carried out six decades ago. Failures were not uncommon in the beginning, leading on to the analysis of the problem and refinements in technique. Improvements in sutures, instrumentation and better microscopes further helped the surgeons to do replantation with better finesse and functional results. Evaluation of results and particularly failure and long term results help the younger surgeons to learn from the difficulties faced earlier to do better in the future. An attempt is made to list various aspects of replantation experienced by the author during the past 30 years, particularly in reference to unfavorable results, which had been occasionally total failure, or a partial failure, with poor function and cosmesis due to infection. An insensate limb with poor function is the result of inadequate or improper nerve coaptation or infection destroying the whole repair. It is apt to mention that infection is mostly the result of poor vascularity due to devitalized tissue. Difficulties arise often in identifying the viable tissue, particularly while debriding in the distal amputated part since there is no bleeding. Experience counts in this, specifically to identify the viable muscle. The factors that may lead to complications are listed with remarks to avoid them.

Evaluation of serpentine ore as a nuclear shielding material using gas chromatographic techniques

International Nuclear Information System (INIS)

Singh, B.N.; Unnikrishnan, E.K.; Kumar, Sangita D.

2007-01-01

Serpentine ore mixed with cement has been recognized as a candidate shielding material for use in nuclear reactors because of its many desirable properties. Therefore the assessment of serpentine ore for release of volatile gases during exposure to elevated temperatures, irradiation and changes in chemical composition, is essential. The present paper deals with the studies on the serpentine ores using gas chromatography and combustion gas chromatographic techniques. (author)

Unfavorable Communications Lead to Conflicts in Building Projects

DEFF Research Database (Denmark)

Ussing, Lene Faber; Wandahl, Søren

2013-01-01

The building industry in Denmark is accused of moving towards a conflict culture. The aim of this survey is, therefore, to investigate how the parties in the building industry experience this. The study answers the following two questions: Can unfavorable communications in a building project team...... of misunderstanding and conflicts depends on the way of communicating, and the degree of trust between the parties in a building project team depends on how familiar the parties are with each other. The results indicate that the building industry has to seek new ways of working together to obtain a better...... communication and more trust to each other....

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.

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)

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.

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.

Prediction of Nanoparticle and Colloid Attachment on Unfavorable Mineral Surfaces Using Representative Discrete Heterogeneity.

Science.gov (United States)

Trauscht, Jacob; Pazmino, Eddy; Johnson, William P

2015-09-01

Despite several decades of research there currently exists no mechanistic theory to predict colloid attachment in porous media under environmental conditions where colloid-collector repulsion exists (unfavorable conditions for attachment). It has long been inferred that nano- to microscale surface heterogeneity (herein called discrete heterogeneity) drives colloid attachment under unfavorable conditions. Incorporating discrete heterogeneity into colloid-collector interaction calculations in particle trajectory simulations predicts colloid attachment under unfavorable conditions. As yet, discrete heterogeneity cannot be independently measured by spectroscopic or other approaches in ways directly relevant to colloid-surface interaction. This, combined with the fact that a given discrete heterogeneity representation will interact differently with differently sized colloids as well as different ionic strengths for a given sized colloid, suggests a strategy to back out representative discrete heterogeneity by a comparison of simulations to experiments performed across a range of colloid size, solution IS, and fluid velocity. This has recently been performed for interaction of carboxylate-modified polystyrene latex (CML) microsphere attachment to soda lime glass at pH 6.7 with NaCl electrolyte. However, extension to other surfaces, pH values, and electrolytes is needed. For this reason, the attachment of CML (0.25, 1.1, and 2.0 μm diameters) from aqueous suspension onto a variety of unfavorable mineral surfaces (soda lime glass, muscovite, and albite) was examined for pH values of 6.7 and 8.0), fluid velocities (1.71 × 10(-3) and 5.94 × 10(-3) m s(-1)), IS (6.0 and 20 mM), and electrolytes (NaCl, CaSO4, and multivalent mixtures). The resulting representative heterogeneities (heterodomain size and surface coverage, where heterodomain refers to nano- to microscale attractive domains) yielded colloid attachment predictions that were compared to predictions from existing

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

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

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 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.

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.

Temperature Control of Gas Chromatograph Based on Switched Delayed System Techniques

Directory of Open Access Journals (Sweden)

Xiao-Liang Wang

2014-01-01

Full Text Available We address the temperature control problem of the gas chromatograph. We model the temperature control system of the gas chromatograph into a switched delayed system and analyze the stability by common Lyapunov functional technique. The PI controller parameters can be given based on the proposed linear matrix inequalities (LMIs condition and the designed controller can make the temperature of gas chromatograph track the reference signal asymptotically. An experiment is given to illustrate the effectiveness of the stability criterion.

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)

State and business co-operation in settling socio-economic issues: forward to sustainable development of ecologically unfavorable regions

Science.gov (United States)

Bashkirova, N. N.; Lessovaia, S. N.

2018-01-01

The complexity of socio-economic issues of mono-cities located in the ecologically unfavorable regions of Eurasia was disclosed. The economically strategic role of city-forming mining enterprises and their impact on ecological situation was revealed. The general conception of settling the socio-economic problems of mono-cities located in ecologically unfavorable regions was worked out. Various approached to the concentration of financial resources for economic and ecological sustainable development of the regions located on the north of Eurasia holding nature protection actions were submitted. Based on performed critical analysis of the positive international experience of ecological taxation some approaches to reforming current Russian system of ecological taxation were suggested. It was revealed that increasing the social responsibilities of business in the field of waste recycling, environmental protection and monitoring of ecological conditions of territories and state and business co-operation are the most efficient opportunities in settling socio-economic issues of ecologically unfavorable regions.

A chromatographic study of the Lewis acid-base chemistry of zirconia surfaces

International Nuclear Information System (INIS)

Blackwell, J.A.; Carr, P.W.

1991-01-01

This paper reports on the chromatographic properties of porous microparticulate zirconium oxide surfaces in aqueous media which are highly dependent upon the chemical composition of the eluent. In particular, retention is controlled by the type and concentration of hard Ligand exchange is the dominant mechanism for the retention of solutes which are Lewis bases. consequently, the capacity factor and plate height depend on both the thermodynamic and kinetic properties of whatever competing Lewis bases may be present in the eluent. These Lewis base eluent components act to control retention in two ways. They modify the net ligand exchange contribution to retention, and they serve as sites for secondary interactions, such as hydrogen bonding and hydrophobic interactions between solutes and the dynamic stationary phase

Total Delay Is Associated with Unfavorable Treatment Outcome among Pulmonary Tuberculosis Patients in West Gojjam Zone, Northwest Ethiopia: A Prospective Cohort Study.

Directory of Open Access Journals (Sweden)

Senedu Bekele Gebreegziabher

Full Text Available delay in diagnosis and treatment of tuberculosis (TB may worsen the disease, increase mortality and enhance transmission in the community. This study aimed at assessing the association between total delay and unfavorable treatment outcome among newly diagnosed pulmonary TB (PTB patients.A prospective cohort study was conducted in West Gojjam Zone, Amhara Region of Ethiopia from October 2013 to May 2015. Newly diagnosed PTB patients who were ≥15 years of age were consecutively enrolled in the study from 30 randomly selected public health facilities. Total delay (the time period from onset of TB symptoms to first start of anti-TB treatment was measured. Median total delay was calculated. Mixed effect logistics regression was used to analyze factors associated with unfavorable treatment outcome.Seven hundred six patients were enrolled in the study. The median total delay was 60 days. Patients with total delay of > 60 days were more likely to have unfavorable TB treatment outcome than patients with total delay of ≤ 60 days (adjusted odds ratio [AOR], 2.33; 95% confidence interval [CI], 1.04-5.26. Human immunodeficiency virus (HIV positive TB patients were 8.46 times more likely to experience unfavorable treatment outcome than HIV negative TB patients (AOR, 8.46; 95% CI, 3.14-22.79.Long total delay and TB/HIV coinfection were associated with unfavorable treatment outcome. Targeted interventions that can reduce delay in diagnosis and treatment of TB, and early comprehensive management of TB/HIV coinfection are needed to reduce increased risk of unfavorable treatment outcome.

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

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

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.

Postdates induction with an unfavorable cervix and risk of cesarean.

Science.gov (United States)

McCoy, Jennifer; Downes, Katheryne L; Srinivas, Sindhu K; Levine, Lisa D

2018-03-21

To determine the risk of cesarean delivery associated with postdates induction (≥41 weeks) compared to term induction (37-40w6d) among women with an unfavorable cervix, and to examine the risk factors associated with cesarean among women undergoing postdates induction. A planned secondary analysis of a large prospective cohort study on induction (n = 854) was performed. Women with a singleton gestation, intact membranes, and an unfavorable cervix (Bishop score of ≤6 and dilation ≤2 cm) who were undergoing a term (≥37 weeks) induction for any indication were included. Women with a prior cesarean were excluded. The primary outcome was cesarean delivery. Relative risk of cesarean was estimated using a modified Poisson's regression model. There was a significantly increased risk of cesarean for women undergoing postdates induction (n = 154) compared to women 37-40w6d (n = 700), (46.8 versus 26.0%, p cesarean remained after adjustment for race, parity, and pregnancy-related hypertension (aRR 1.70 [1.39-2.09], p cesarean among women ≥41 weeks included nulliparity (aRR 3.38 95%CI (2.42-4.74)), BMI ≥30 (aRR 1.72 95%CI (1.34-2.21)), and starting cervical dilation cesarean compared to women 37-40w6d, with nulliparity, obesity, and cervical dilation <1 cm being independent risk factors. These data can be used to augment patient counseling and support the ongoing discussion regarding the risk of post dates induction.

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.

Hamsi scoring in the prediction of unfavorable outcomes from tuberculous meningitis

DEFF Research Database (Denmark)

Erdem, Hakan; Ozturk-Engin, Derya; Tireli, Hulya

2015-01-01

, hydrocephalus, vasculitis, immunosuppression, diabetes mellitus and neurological deficit remained in the final model. Scores 1-3 were assigned to the variables in the severity scale, which included scores of 1-6. The distribution of mortality for the scores 1-6 was 3.4, 8.2, 20.6, 31, 30 and 40.1%, respectively....... Altered consciousness, diabetes mellitus, immunosuppression, neurological deficits, hydrocephalus, and vasculitis predicted the unfavorable outcome in the scoring and the cumulative score provided a linear estimation of prognosis....

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)

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.

Unfavorably Altered Fibrin Clot Properties in Patients with Eosinophilic Granulomatosis with Polyangiitis (Churg-Strauss Syndrome): Association with Thrombin Generation and Eosinophilia.

Science.gov (United States)

Mastalerz, Lucyna; Celińska-Lӧwenhoff, Magdalena; Krawiec, Piotr; Batko, Bogdan; Tłustochowicz, Witold; Undas, Anetta

2015-01-01

Given reports on the increased prevalence of thromboembolic incidents in patients with eosinophilic granulomatosis with polyangiitis (EGPA; Churg-Strauss syndrome), we investigated whether fibrin clot properties are unfavorably altered in EGPA. Ex vivo plasma fibrin clot characteristics, including clot permeability, turbidimetry and efficiency of fibrinolysis using two assays, were investigated in 34 consecutive patients with remission in EGPA according to the Birmingham Vasculitis Activity Score version 3 (23 female, 11 male), aged 48 (range, 21-80) years. The control group comprised 34 age- and sex- matched volunteers. Compared with controls, patients with EGPA were characterized by denser fiber clots (estimated pore size, Ks, 7.30±0.93 vs 10.14±1.07 10-9 cm2), faster fibrin polymerization (lag phase in a turbidimetric curve, 41.8±3.6 vs 47.4±2.9 s), thicker fibrin fibers (maximum absorbance, ΔAbs, 0.87±0.09 vs 0.72±0.07), higher maximum levels of D-dimer released from clots (DDmax 4.10±0.46 vs 3.54±0.35 mg/L), and prolonged clot lysis time (t50%; 9.50±1.45 vs 7.56±0.87 min); all p<0.0001. Scanning electron microscopy images confirmed denser plasma fibrin networks composed of thinner fibers formed in EGPA. Antineutrophil cytoplasmic antibody status and C-reactive protein did not affect clot variables. Multivariate analysis adjusted for fibrinogen showed that Ks was predicted by eosinophil count, peak thrombin generation, factor VIII, and soluble CD40 ligand, whereas eosinophil count, peak thrombin generation and antiplasmin predicted t50%. This study is the first to show that EGPA is associated with prothrombotic plasma fibrin clot phenotype, which may contribute to thromboembolic manifestations reported in this disease.

Unfavorably Altered Fibrin Clot Properties in Patients with Eosinophilic Granulomatosis with Polyangiitis (Churg-Strauss Syndrome: Association with Thrombin Generation and Eosinophilia.

Directory of Open Access Journals (Sweden)

Lucyna Mastalerz

Full Text Available Given reports on the increased prevalence of thromboembolic incidents in patients with eosinophilic granulomatosis with polyangiitis (EGPA; Churg-Strauss syndrome, we investigated whether fibrin clot properties are unfavorably altered in EGPA.Ex vivo plasma fibrin clot characteristics, including clot permeability, turbidimetry and efficiency of fibrinolysis using two assays, were investigated in 34 consecutive patients with remission in EGPA according to the Birmingham Vasculitis Activity Score version 3 (23 female, 11 male, aged 48 (range, 21-80 years. The control group comprised 34 age- and sex- matched volunteers.Compared with controls, patients with EGPA were characterized by denser fiber clots (estimated pore size, Ks, 7.30±0.93 vs 10.14±1.07 10-9 cm2, faster fibrin polymerization (lag phase in a turbidimetric curve, 41.8±3.6 vs 47.4±2.9 s, thicker fibrin fibers (maximum absorbance, ΔAbs, 0.87±0.09 vs 0.72±0.07, higher maximum levels of D-dimer released from clots (DDmax 4.10±0.46 vs 3.54±0.35 mg/L, and prolonged clot lysis time (t50%; 9.50±1.45 vs 7.56±0.87 min; all p<0.0001. Scanning electron microscopy images confirmed denser plasma fibrin networks composed of thinner fibers formed in EGPA. Antineutrophil cytoplasmic antibody status and C-reactive protein did not affect clot variables. Multivariate analysis adjusted for fibrinogen showed that Ks was predicted by eosinophil count, peak thrombin generation, factor VIII, and soluble CD40 ligand, whereas eosinophil count, peak thrombin generation and antiplasmin predicted t50%.This study is the first to show that EGPA is associated with prothrombotic plasma fibrin clot phenotype, which may contribute to thromboembolic manifestations reported in this disease.

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 ...

Chromatographic profiles of extractives from leaves of Eugenia uniflora

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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.

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.

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.

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

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

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...

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.

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

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

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

A simple subcritical chromatographic test for an extended ODS high performance liquid chromatography column classification.

Science.gov (United States)

Lesellier, Eric; Tchapla, Alain

2005-12-23

This paper describes a new test designed in subcritical fluid chromatography (SFC) to compare the commercial C18 stationary phase properties. This test provides, from a single analysis of carotenoid pigments, the absolute hydrophobicity, the silanol activity and the steric separation factor of the ODS stationary phases. Both the choice of the analytical conditions and the validation of the information obtained from the chromatographic measurements are detailed. Correlations of the carotenoid test results with results obtained from other tests (Tanaka, Engelhard, Sander and Wise) performed both in SFC and HPLC are discussed. Two separation factors, calculated from the retention of carotenoid pigments used as probe, allowed to draw a first classification diagram. Columns, which present identical chromatographic behaviors are located in the same area on this diagram. This location can be related to the stationary phase properties: endcapping treatments, bonding density, linkage functionality, specific area or silica pore diameter. From the first classification, eight groups of columns are distinguished. One group of polymer coated silica, three groups of polymeric octadecyl phases, depending on the pore size and the endcapping treatment, and four groups of monomeric stationary phases. An additional classification of the four monomeric groups allows the comparison of these stationary phases inside each group by using the total hydrophobicity. One hundred and twenty-nine columns were analysed by this simple and rapid test, which allows a comparison of columns with the aim of helping along their choice in HPLC.

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.

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+.

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.

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.

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.)

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.

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

Transfer points of belt conveyors operating with unfavorable bulk

Energy Technology Data Exchange (ETDEWEB)

Goehring, H [Technische Universitaet, Dresden (German Democratic Republic)

1989-06-01

Describes design of belt conveyor chutes that transfer bulk of surface mines from one conveyor to another. Conveyor belt velocity is a significant parameter. Unfavorable chute design may lead to bulk flow congestion, bulk velocity losses etc. The bulk flow process is analyzed, bulk flow velocities, belt inclinations and bulk feeding from 2 conveyors into one chute are taken into account. Conventional chutes have parabolic belt impact walls. An improved version with divided impact walls is proposed that maintains a relatively high bulk velocity, reduces friction at chute walls and decreases wear and dirt build-up. Design of the improved chute is explained. It is built to adapt to existing structures without major modifications. The angle between 2 belt conveyors can be up to 90 degrees, the best bulk transfer is noted at conveyor angles below 60 degrees. Various graphs and schemes are provided. 6 refs.

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.

[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.

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.

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 ...

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.

Case Study: Unfavorable But Transient Physiological Changes During Contest Preparation in a Drug-Free Male Bodybuilder.

Science.gov (United States)

Pardue, Andrew; Trexler, Eric T; Sprod, Lisa K

2017-12-01

Extreme body composition demands of competitive bodybuilding have been associated with unfavorable physiological changes, including alterations in metabolic rate and endocrine profile. The current case study evaluated the effects of contest preparation (8 months), followed by recovery (5 months), on a competitive drug-free male bodybuilder over 13 months (M1-M13). Serum testosterone, triiodothyronine (T 3 ), thyroxine (T 4 ), cortisol, leptin, and ghrelin were measured throughout the study. Body composition (BodPod, dualenergy x-ray absorptiometry [DXA]), anaerobic power (Wingate test), and resting metabolic rate (RMR) were assessed monthly. Sleep was assessed monthly via the Pittsburgh Sleep Quality Index (PSQI) and actigraphy. From M1 to M8, testosterone (623-173 ng∙dL -1 ), T 3 (123-40 ng∙dL -1 ), and T 4 (5.8-4.1 mg∙dL -1 ) decreased, while cortisol (25.2-26.5 mg∙dL -1 ) and ghrelin (383-822 pg∙mL -1 ) increased. The participant lost 9.1 kg before competition as typical energy intake dropped from 3,860 to 1,724 kcal∙day -1 ; BodPod estimates of body fat percentage were 13.4% at M1, 9.6% at M8, and 14.9% at M13; DXA estimates were 13.8%, 5.1%, and 13.8%, respectively. Peak anaerobic power (753.0 to 536.5 Watts) and RMR (107.2% of predicted to 81.2% of predicted) also decreased throughout preparation. Subjective sleep quality decreased from M1 to M8, but objective measures indicated minimal change. By M13, physiological changes were largely, but not entirely, reversed. Contest preparation may yield transient, unfavorable changes in endocrine profile, power output, RMR, and subjective sleep outcomes. Research with larger samples must identify strategies that minimize unfavorable adaptations and facilitate recovery following competition.

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.

Influence of Fatty Acid Methyl Esters on Fuel properties of Biodiesel ...

African Journals Online (AJOL)

Influence of Fatty Acid Methyl Esters on Fuel properties of Biodiesel Produced from the. Seeds Oil of Curcubita ... Gas chromatograph coupled with mass spectrophotometer (GC-MS). The results indicate ..... Chemical and physical properties of ...

Preparation of porous hollow silica spheres via a layer-by-layer process and the chromatographic performance

Science.gov (United States)

Wei, Xiaobing; Gong, Cairong; Chen, Xujuan; Fan, Guoliang; Xu, Xinhua

2017-03-01

Hollow silica spheres possessing excellent mechanical properties were successfully prepared through a layer-by-layer process using uniform polystyrene (PS) latex fabricated by dispersion polymerization as template. The formation of hollow SiO2 micro-spheres, structures and properties were observed in detail by zeta potential, SEM, TEM, FTIR, TGA and nitrogen sorption porosimetry. The results indicated that the hollow spheres were uniform with particle diameter of 1.6 μm and shell thickness of 150 nm. The surface area was 511 m2/g and the pore diameter was 8.36 nm. A new stationary phase for HPLC was obtained by using C18-derivatized hollow SiO2 micro-spheres as packing materials and the chromatographic properties were evaluated for the separation of some regular small molecules. The packed column showed low column pressure, high values of efficiency (up to about 43 000 plates/m) and appropriate asymmetry factors.

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)

Light ion irradiation for unfavorable soft tissue sarcoma

International Nuclear Information System (INIS)

Linstadt, D.; Castro, J.R.; Phillips, T.L.; Petti, P.L.; Collier, J.M.; Daftari, I.; Schoethaler, R.; Rayner, A.

1990-09-01

Between 1978 and 1989, 32 patients with unfavorable soft tissue sarcoma underwent light ion (helium, neon) irradiation with curative intent at Lawrence Berkeley Laboratory. The tumors were located in the trunk in 22 patients and head and neck in 10. Macroscopic tumor was present in 22 at the time of irradiation. Two patients had tumors apparently induced by previous therapeutic irradiation. Follow-up times for surviving patients ranged from 4 to 121 months (median 27 months). The overall 3-year actuarial local control rate was 62%; the corresponding survival rate was 50%. The 3-year actuarial control rate for patients irradiated with macroscopic tumors was 48%, while none of the patients with microscopic disease developed local recurrence (100%). The corresponding 3-year actuarial survival rates were 40% (macroscopic) and 78% (microscopic). Patients with retroperitoneal sarcoma did notably well; the local control rate and survival rate were 64% and 62%, respectively. Complications were acceptable; there were no radiation related deaths, while two patients (6%) required operations to correct significant radiation-related injuries. These results appear promising compared to those achieved by low -LET irradiation, and suggest that this technique merits further investigation

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

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.

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.

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) ...

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....

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...

Double microcatheter technique for coiling intracranial aneurysms with unfavorable configurations

Directory of Open Access Journals (Sweden)

WANG Shu-yuan

2013-03-01

Full Text Available Background Although stent-assisted technique has been widely used clinically, it is still hard to perform coiling treatment for complicated intracranial aneurysms, including relatively wide-necked tiny aneurysms and lobulated wide-necked aneurys ms with important branch vessels arising from the neck. This study aims to investigate the feasibility and clinical results of endovascular treatment for intracranial aneurysms with unfavorable configurations by using double microcatheter technique. Methods Thirty-three cases with complicated aneurysms were treated by using double microcatheter technique from April 2008 to November 2012. The locations of these aneurysms were anterior communicating artery (7 cases, posterior communicating artery (14 cases, ophthalmic artery (3 cases, anterior choroidal artery (3 cases, origin of posterior inferior cerebellar artery (3 cases, bifurcation of middle cerebral artery (2 cases and top of basilar artery (1 case. The mean neck- to-body (width ratio was 0.80 ± 0.21 (0.53-1.33. The mean body (width-to-dome (height ratio was 1.12 ± 0.37 (0.55-2.12. The mean dome (height-to-neck ratio was 1.26 ± 0.41 (0.65-2.96. The diameter of neck ≥4 mm was seen in 7 aneurysms, neck≥height in 9 and neck ≥width in 8. Besides, there were 9 very small aneurysms (the maximum diameter≤3 mm and 13 aneurysms with important branch vessels arising from the neck. All of these aneurysms were treated with coiling by using double microcatheter technique. Results All aneurysms were successfully embolized. Immediate postembolization angiography showed no residual contrast filling in 19 aneurysms, and residual filling in 14. There were some small loops protruding from the neck without influencing the blood flow in 12 cases. At discharge, according to modified Rankin Scale (mRS, 30 patients with 0-1 scores presented excellent clinical outcomes and 3 patients with 2 scores had cognitive dysfunction and moderate disability due to vasospasm

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.

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 ...

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)

[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.

Chromatographic Characterization and GC-MS Evaluation of the Bioactive Constituents with Antimicrobial Potential from the Pigmented Ink of Loligo duvauceli

OpenAIRE

Girija, Smiline; Duraipandiyan, Veeramuthu; Kuppusamy, Pandi Suba; Gajendran, Hariprasad; Rajagopal, Raghuraman

2014-01-01

Chromatographic characterization and the GC-MS evaluation of the black pigmented ink of Loligo duvauceli in the present study have yielded an array of bioactive compounds with potent antimicrobial property. Facing an alarm of antimicrobial resistance globally, a need for elucidating antimicrobial agents from natural sources will be the need for the hour. In this view, this study is aimed at characterizing the black pigmented ink of the Indian squid L. duvauceli. The squid ink was subjected to...

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

[Determination of priority unfavorable environmental factors].

Science.gov (United States)

Zaikova, Z A; Burdukovskaya, A V; Belykh, A I

In the Irkutsk region there are recorded high indices of rates of morbidity, disability, mortality rate of the working-age population and low levels of life expectancy of the population, that is confirmed by ranking position levels among the all subjects of the Russian Federation. According to all mentioned indices of health the region is inside the top ten unfavorable regions of Russia. In relation to the problem in the state of health of the adult population the estimation of the causal relationships between environmental factors and certain health indices is actual. The list of studiedfactors included health indices that characterize the harmful working conditions of the working population and basic socioeconomic indices in the region. Estimation of causal-relationship relationships was performed with the use of methods of multivariate analysis - correlation and multiple linear regression. In the selection offactors for the construction of mathematical models of multiple regression there were used methods of the analysis of variables variability, pair correlation coefficients matrix and sequential switching covariates to eliminate the problems of multicollinearity, pre-standardization of indices for the elevation of the numerical stability of regression analysis algorithm. As a result of the execution of the analysis there were constructed statistical models for the dependence in the system variables “environment - public health”, which allowed to identify the most informative regression models for the adult population health according to indices of primary disability of the population, the mortality rate and life expectancy of the working age population. According to results of the analysis there were identified priority factors affecting on the health of the adult population of the Irkutsk region. To these factors there are referred the proportion of workplaces failing to meet sanitary standards for vibration and 8 socio-economic indices of living

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.

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

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

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.

The employment of cellulose pressure columns for the chromatographic separation of radioactive nuclides

International Nuclear Information System (INIS)

Meier, H.; Zimmerhackl, E.; Unger, E.; Zeitler, G.; Albrecht, W.; Boesche, D.; Hecker, W.; Menge, P.

1975-01-01

A study was made of the separation properties of cellulose pressure columns operating at a slight over-pressure of around 1 atmosphere, with respect to the length of the column packing, the flow rate, and the load. The optimal separation stage heights of the columns are situated at H=0.16 mm. Since as a consequence of the favorable separation stage heights observed at column lengths of 3 to 7 cm, separation stage numbers of 200 to 400 are attained, and hence it is possible to attain separations within several minutes with flow rates of 1 ml/min. The choice of the mobile phase is made easier by the fact that paper chromatographic Rsub(f)-values can be transferred to the cellulose pressure column with the aid of a transfer function. (author)

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.

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

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.

Estimation for Retention Factor of Isoflavones in Physico-Chemical Properties

International Nuclear Information System (INIS)

Lee, Seung Ki; Row, Kyung Ho

2003-01-01

The estimation of retention factors by correlation equations with physico-chmical properties maybe helpful in chromatographic work. The physico-chemical properties were water solubility (S), hydrophobicity (P), total energy (Et), connectivity index 1 (1χ), hydrophilic-lipophlic balance (x) and hydrophilic surface area (h) of isoflavones. The retention factors were experimentally measured by RP-HPLC. Especially, the empirical regulations of water solubility and hydrophobicity were expressed in a linear form. The equation between retention factors and various physico-chemical properties of isoflavones was suggested as k = a0 + a 1 log S + a2 log P Q + a3 (E t ) + a4 ( 1 χ) + a5 (x) + a6 (h), and the correlation coefficients estimated were relatively higher than 0.95. The empirical equations might be successfully used for a prediction of the various chromatographic characteristics of substances, with a similar chemical structure

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.

Malnutrition associated with unfavorable outcome and death among South African MDR-TB and HIV co-infected children.

Science.gov (United States)

Hicks, R M; Padayatchi, N; Shah, N S; Wolf, A; Werner, L; Sunkari, V B; O'Donnell, M R

2014-09-01

Pediatric multidrug-resistant tuberculosis (MDR-TB) is complicated by difficult diagnosis, complex treatment, and high mortality. In South Africa, these challenges are amplified by human immunodeficiency virus (HIV) co-infection; however, evidence on treatment outcomes among co-infected children is limited. Using conventional and new pediatric definitions, to describe treatment outcomes and identify risk factors for unfavorable outcome and mortality in children aged children (median age 8 years, IQR 4-12) with MDR-TB (n = 78) or XDR-TB (n = 6) initiated treatment. Sixty-four (77%) were HIV-positive and 62 (97%) received antiretroviral therapy. Sixty-six (79%) achieved favorable treatment outcomes. Overall mortality was 11% (n = 9) at 18 months after initiation of treatment. Malnutrition (aOR 27.4, 95%CI 2.7-278.7) and severe radiographic findings (aOR 4.68, 95%CI 1.01-21.9) were associated with unfavorable outcome. New pediatric outcome definitions increased the proportion classified as cured. It is possible to successfully treat pediatric MDR-TB-HIV even in resource-poor settings. Malnutrition is a marker for severe TB-HIV disease, and is a potential target for future interventions in these patients.

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

Energetically Unfavorable Amide Conformations for N6-Acetyllysine Side Chains in Refined Protein Structures

Science.gov (United States)

Genshaft, Alexander; Moser, Joe-Ann S.; D'Antonio, Edward L.; Bowman, Christine M.; Christianson, David W.

2013-01-01

The reversible acetylation of lysine to form N6-acetyllysine in the regulation of protein function is a hallmark of epigenetics. Acetylation of the positively charged amino group of the lysine side chain generates a neutral N-alkylacetamide moiety that serves as a molecular “switch” for the modulation of protein function and protein-protein interactions. We now report the analysis of 381 N6-acetyllysine side chain amide conformations as found in 79 protein crystal structures and 11 protein NMR structures deposited in the Protein Data Bank (PDB) of the Research Collaboratory for Structural Bioinformatics. We find that only 74.3% of N6-acetyllysine residues in protein crystal structures and 46.5% in protein NMR structures contain amide groups with energetically preferred trans or generously trans conformations. Surprisingly, 17.6% of N6-acetyllysine residues in protein crystal structures and 5.3% in protein NMR structures contain amide groups with energetically unfavorable cis or generously cis conformations. Even more surprisingly, 8.1% of N6-acetyllysine residues in protein crystal structures and 48.2% in NMR structures contain amide groups with energetically prohibitive twisted conformations that approach the transition state structure for cis-trans isomerization. In contrast, 109 unique N-alkylacetamide groups contained in 84 highly-accurate small molecule crystal structures retrieved from the Cambridge Structural Database exclusively adopt energetically preferred trans conformations. Therefore, we conclude that cis and twisted N6-acetyllysine amides in protein structures deposited in the PDB are erroneously modeled due to their energetically unfavorable or prohibitive conformations. PMID:23401043

Radiation therapy for Kasabach-Merritt syndrome. Analysis of unfavorable factors in 5 children

International Nuclear Information System (INIS)

Kawamori, Jiro; Saito, Tsutomu; Tanaka, Yoshiaki; Sato, Katsuhiko.

1996-01-01

During the past 10 years, five infants with Kasabach-Merritt syndrome (K-M) receiving radiation therapy were reported. We investigated whether radiation therapy for K-M was useful and what the unfavorable factors of K-M were. During the past 10 years, we have treated five infants with K-M. The syndrome occurred at ages ranging from birth to 4 months. The incidence of female to male ratio was 3:2. Among 5 cases, the site of hemangioma was as follows; shoulder, anterior chest wall, lower abdominal wall, face and neck and inguinal site. All 5 cases received medication to control the coagulopathy including prednisone and blood transfusion at first. Because the platelet count and the bleeding tendency did not improve in any case, these cases received radiation therapy. Total dose ranged from 5 to 10 Gy and fraction-size ranged from 0.5 to 1.75 Gy. Irradiation session was 2 or 3 times per week. In 5 cases, 4 cases showed cure of bleeding tendency and disappearance of tumor, and survived. In these 4 cases, normalization of platelet count was obtained at the early phase of dose ranging from 3 to 5 Gy by radiation therapy. In the remaining case, bleeding tendency was improved at the late phase by initial radiation therapy, however, after that immediately relapsed. In this case, the salvage radiation therapy was not effective and she died from airway obstruction. This case was of neonatal age and had bulky neck tumor. We recognized that radiation therapy was effective for K-M. A serious case was of neonatal age and had bulky neck tumor. It was estimated that the unfavorable factors of K-M were neonatal case and bulky neck tumor case. (author)

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.

Anatomy of the bovine ascending aorta and brachiocephalic artery found unfavorable for total artificial heart implant.

Science.gov (United States)

Karimov, Jamshid H; Sunagawa, Gengo; Such, Kimberly A; Sale, Shiva; Golding, Leonard A R; Moazami, Nader; Fukamachi, Kiyotaka

2015-12-01

The biocompatibility assessment of the Cleveland Clinic continuous-flow total artificial heart is an important part of the device developmental program. Surgical and postoperative management are key factors in achieving optimal outcomes. However, the presence of vascular anatomical abnormalities in experimental animal models is often unpredictable and may worsen the expected outcomes. We report a technical impediment encountered during total artificial heart implantation complicated by unfavorable bovine anatomy of the ascending aorta and brachiocephalic arterial trunk.

Influence of thermodynamically unfavorable secondary structures on DNA hybridization kinetics

Science.gov (United States)

Hata, Hiroaki; Kitajima, Tetsuro

2018-01-01

Abstract Nucleic acid secondary structure plays an important role in nucleic acid–nucleic acid recognition/hybridization processes, and is also a vital consideration in DNA nanotechnology. Although the influence of stable secondary structures on hybridization kinetics has been characterized, unstable secondary structures, which show positive ΔG° with self-folding, can also form, and their effects have not been systematically investigated. Such thermodynamically unfavorable secondary structures should not be ignored in DNA hybridization kinetics, especially under isothermal conditions. Here, we report that positive ΔG° secondary structures can change the hybridization rate by two-orders of magnitude, despite the fact that their hybridization obeyed second-order reaction kinetics. The temperature dependence of hybridization rates showed non-Arrhenius behavior; thus, their hybridization is considered to be nucleation limited. We derived a model describing how ΔG° positive secondary structures affect hybridization kinetics in stopped-flow experiments with 47 pairs of oligonucleotides. The calculated hybridization rates, which were based on the model, quantitatively agreed with the experimental rate constant. PMID:29220504

Adsorption and gas-chromatographic properties of tungsten selenide

International Nuclear Information System (INIS)

Gavrilova, T.B.; Kiselev, A.V.; Roshchina, T.M.

1988-01-01

Method of gas chromatography was used to investigate the surface properties of a series of tungsten selenide WSe 2 samples as well as to determine the role of geometrical and electronic structure of adsorbate molecules and their orientation with respect to the surface during adsorption on WSe 2 . Thermodynamic characteristics of hydrocarbon C 6 -C 10 adsorption at surface occupation close to the zero one were determined. Correlation of the values of thermodynamic characteristics of saturated and aromatic hydrocarbon adsorption enabled to refer WSe 2 to nonspecific adsorbents. It is noted that the main role during hydrocarbon adsorption on WSe 2 is played by nonpolar basic facets, occupied by selenium atoms

Measurement of water absorption capacity in wheat flour by a headspace gas chromatographic technique.

Science.gov (United States)

Xie, Wei-Qi; Yu, Kong-Xian; Gong, Yi-Xian

2018-04-17

The purpose of this work is to introduce a new method for quantitatively analyzing water absorption capacity in wheat flour by a headspace gas chromatographic technique. This headspace gas chromatographic technique was based on measuring the water vapor released from a series of wheat flour samples with different contents of water addition. According to the different trends between the vapor and wheat flour phase before and after the water absorption capacity in wheat flour, a turning point (corresponding to water absorption capacity in wheat flour) can be obtained by fitting the data of the water gas chromatography peak area from different wheat flour samples. The data showed that the phase equilibrium in the vial can be achieved in 25 min at desired temperature (35°C). The relative standard deviation of the reaction headspace gas chromatographic technique in water absorption capacity determination was within 3.48%, the relative differences has been determined by comparing the water absorption capacity obtained from this new analytical technique with the data from the reference technique (i.e., the filtration method), which are less than 8.92%. The new headspace gas chromatographic method is automated, accurate and be a reliable tool for quantifying water absorption capacity in wheat flour in both laboratory research and mill applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Deposition and reentrainment of Brownian particles in porous media under unfavorable chemical conditions: some concepts and applications.

Science.gov (United States)

Hahn, Melinda W; O'Meliae, Charles R

2004-01-01

The deposition and reentrainment of particles in porous media have been examined theoretically and experimentally. A Brownian Dynamics/Monte Carlo (MC/BD) model has been developed that simulates the movement of Brownian particles near a collector under "unfavorable" chemical conditions and allows deposition in primary and secondary minima. A simple Maxwell approach has been used to estimate particle attachment efficiency by assuming deposition in the secondary minimum and calculating the probability of reentrainment. The MC/BD simulations and the Maxwell calculations support an alternative view of the deposition and reentrainment of Brownian particles under unfavorable chemical conditions. These calculations indicate that deposition into and subsequent release from secondary minima can explain reported discrepancies between classic model predictions that assume irreversible deposition in a primary well and experimentally determined deposition efficiencies that are orders of magnitude larger than Interaction Force Boundary Layer (IFBL) predictions. The commonly used IFBL model, for example, is based on the notion of transport over an energy barrier into the primary well and does not address contributions of secondary minimum deposition. A simple Maxwell model based on deposition into and reentrainment from secondary minima is much more accurate in predicting deposition rates for column experiments at low ionic strengths. It also greatly reduces the substantial particle size effects inherent in IFBL models, wherein particle attachment rates are predicted to decrease significantly with increasing particle size. This view is consistent with recent work by others addressing the composition and structure of the first few nanometers at solid-water interfaces including research on modeling water at solid-liquid interfaces, surface speciation, interfacial force measurements, and the rheological properties of concentrated suspensions. It follows that deposition under these

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

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.

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.

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.

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.

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.

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)

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.

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.

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.)

Dose escalation using conformal high-dose-rate brachytherapy improves outcome in unfavorable prostate cancer.

Science.gov (United States)

Martinez, Alvaro A; Gustafson, Gary; Gonzalez, José; Armour, Elwood; Mitchell, Chris; Edmundson, Gregory; Spencer, William; Stromberg, Jannifer; Huang, Raywin; Vicini, Frank

2002-06-01

To overcome radioresistance for patients with unfavorable prostate cancer, a prospective trial of pelvic external beam irradiation (EBRT) interdigitated with dose-escalating conformal high-dose-rate (HDR) prostate brachytherapy was performed. Between November 1991 and August 2000, 207 patients were treated with 46 Gy pelvic EBRT and increasing HDR brachytherapy boost doses (5.50-11.5 Gy/fraction) during 5 weeks. The eligibility criteria were pretreatment prostate-specific antigen level >or=10.0 ng/mL, Gleason score >or=7, or clinical Stage T2b or higher. Patients were divided into 2 dose levels, low-dose biologically effective dose 93 Gy (149 patients). No patient received hormones. We used the American Society for Therapeutic Radiology and Oncology definition for biochemical failure. The median age was 69 years. The mean follow-up for the group was 4.4 years, and for the low and high-dose levels, it was 7.0 and 3.4 years, respectively. The actuarial 5-year biochemical control rate was 74%, and the overall, cause-specific, and disease-free survival rate was 92%, 98%, and 68%, respectively. The 5-year biochemical control rate for the low-dose group was 52%; the rate for the high-dose group was 87% (p failure. The Radiation Therapy Oncology Group Grade 3 gastrointestinal/genitourinary complications ranged from 0.5% to 9%. The actuarial 5-year impotency rate was 51%. Pelvic EBRT interdigitated with transrectal ultrasound-guided real-time conformal HDR prostate brachytherapy boost is both a precise dose delivery system and a very effective treatment for unfavorable prostate cancer. We demonstrated an incremental beneficial effect on biochemical control and cause-specific survival with higher doses. These results, coupled with the low risk of complications, the advantage of not being radioactive after implantation, and the real-time interactive planning, define a new standard for treatment.

Grouting techniques for the unfavorable geological conditions of Xiang'an subsea tunnel in China

Directory of Open Access Journals (Sweden)

Dingli Zhang

2014-10-01

Full Text Available One of the major challenges during subsea tunnel construction is to seal the potential water inflow. The paper presents a case study of Xiang'an subsea tunnel in Xiamen, the first subsea tunnel in China. During its construction, different grades of weathered geomaterials were encountered, which was the challenging issue for this project. To deal with these unfavorable geological conditions, grouting was adopted as an important measure for ground treatment. The grouting mechanism is first illustrated by introducing a typical grouting process. Then the site-specific grouting techniques employed in the Xiang'an subsea tunnel are elaborated. By using this ground reinforcement technique, the tunneling safety of the Xiang'an subsea tunnel was guaranteed.

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

Titanium dioxide as chemo-affinity chromatographic sorbent of biomolecular compounds - Applications in acidic modification-specific proteomics

DEFF Research Database (Denmark)

Engholm-Keller, Kasper; Larsen, Martin R

2011-01-01

biomolecules due to its unique ion and ligand exchange properties and high stability towards pH and temperature. Recently, titanium dioxide chromatography was introduced in proteomics as a highly specific method for enriching phosphorylated peptides - a method, which has been widely adapted by the field...... matrices for further characterization is affinity chromatography, which relies on the specific interaction between an analyte in solution and a solid adsorbent. Titanium dioxide-based affinity chromatography has proven to be a versatile tool in enrichment of various compounds such as phosphorylated....... The development of TiO(2)-based chromatographic strategies for separation of various biomolecules from its introduction for small molecules more than 20years ago until recent proteomics applications today will be reviewed here....

Leaf-level carbon isotope discrimination and its relationship with yield components as a tool for cotton phenotyping in unfavorable conditions

Directory of Open Access Journals (Sweden)

Giovani Greigh Brito

2014-07-01

Full Text Available The initial goal of this study was to measure the efficiency of carbon isotope discrimination (Δ in distinguishing between cotton plant genotypes subjected to two water regimes. In addition, ∆ measurements, leaf water potential and gas exchange ratios were monitored. Using Brazilian breeding lines, this study also tested the usability of ∆ as a proxy for selecting high-performing yield components in cotton plants grown in unfavorable conditions, particularly water deficiency. For these experiments, ∆ and yield components were measured and their correlations analyzed. Differences among cotton genotypes for Δ (p < 0.0001 were verified, and it was found that this variable was significantly correlated with gas exchange. There was a significant positive correlation between Δ and seed cotton yield only in the site experiencing severe water deficiency (Santa Helena de Goiás. However, Δ had a significant negative correlation with fiber percentage. Our results indicate that Δ is a suitable tool for cotton phenotyping, and it may be applied in cotton breeding programs that aim to produce high-performing yield components in unfavorable conditions.

Standard Format for Chromatographic-polarimetric System small samples assessment

International Nuclear Information System (INIS)

Naranjo, S.; Fajer, V.; Fonfria, C.; Patinno, R.

2012-01-01

The treatment of samples containing optically active substances to be evaluated as part of quality control of raw material entering industrial process, and also during the modifications exerted on it to obtain the desired final composition is still and unsolved problem for many industries. That is the case of sugarcane industry. Sometimes the troubles implied are enlarged because samples to be evaluated are not bigger than one milliliter. Reduction of gel beds in G-10 and G-50 chromatographic columns having an inner diameter of 16 mm, instead of 25, and bed heights adjustable to requirements by means of sliding stoppers to increase analytical power were evaluated with glucose and sucrose standards in concentrations from 1 to 10 g/dL, using aliquots of 1 ml without undesirable dilutions that could affect either detection or chromatographic profile. Assays with seaweed extracts gave good results that are shown. It is established the advantage to know concentration of a separated substance by the height of its peak and the savings in time and reagents resulting . Sample expanded uncertainty in both systems is compared. It is also presented several programs for data acquisition, storing and processing. (Author)

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.

QSRR modeling for the chromatographic retention behavior of some β-lactam antibiotics using forward and firefly variable selection algorithms coupled with multiple linear regression.

Science.gov (United States)

Fouad, Marwa A; Tolba, Enas H; El-Shal, Manal A; El Kerdawy, Ahmed M

2018-05-11

The justified continuous emerging of new β-lactam antibiotics provokes the need for developing suitable analytical methods that accelerate and facilitate their analysis. A face central composite experimental design was adopted using different levels of phosphate buffer pH, acetonitrile percentage at zero time and after 15 min in a gradient program to obtain the optimum chromatographic conditions for the elution of 31 β-lactam antibiotics. Retention factors were used as the target property to build two QSRR models utilizing the conventional forward selection and the advanced nature-inspired firefly algorithm for descriptor selection, coupled with multiple linear regression. The obtained models showed high performance in both internal and external validation indicating their robustness and predictive ability. Williams-Hotelling test and student's t-test showed that there is no statistical significant difference between the models' results. Y-randomization validation showed that the obtained models are due to significant correlation between the selected molecular descriptors and the analytes' chromatographic retention. These results indicate that the generated FS-MLR and FFA-MLR models are showing comparable quality on both the training and validation levels. They also gave comparable information about the molecular features that influence the retention behavior of β-lactams under the current chromatographic conditions. We can conclude that in some cases simple conventional feature selection algorithm can be used to generate robust and predictive models comparable to that are generated using advanced ones. Copyright © 2018 Elsevier B.V. All rights reserved.

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. �

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%.

7 CFR Exhibit B-2 to Subpart B of... - Letter for Notifying Applicants, Lenders and Holders and Borrowers of Unfavorable Decision...

Science.gov (United States)

2010-01-01

... and Borrowers of Unfavorable Decision Reached at the Meeting B Exhibit B-2 to Subpart B of Part 1900 Agriculture Regulations of the Department of Agriculture (Continued) RURAL HOUSING SERVICE, RURAL BUSINESS... REGULATIONS GENERAL Adverse Decisions and Administrative Appeals Pt. 1900, Subpt. B, Exh. B-2 Exhibit B-2 to...

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)

Favoring the unfavored: Selective electrochemical nitrogen fixation using a reticular chemistry approach.

Science.gov (United States)

Lee, Hiang Kwee; Koh, Charlynn Sher Lin; Lee, Yih Hong; Liu, Chong; Phang, In Yee; Han, Xuemei; Tsung, Chia-Kuang; Ling, Xing Yi

2018-03-01

Electrochemical nitrogen-to-ammonia fixation is emerging as a sustainable strategy to tackle the hydrogen- and energy-intensive operations by Haber-Bosch process for ammonia production. However, current electrochemical nitrogen reduction reaction (NRR) progress is impeded by overwhelming competition from the hydrogen evolution reaction (HER) across all traditional NRR catalysts and the requirement for elevated temperature/pressure. We achieve both excellent NRR selectivity (~90%) and a significant boost to Faradic efficiency by 10 percentage points even at ambient operations by coating a superhydrophobic metal-organic framework (MOF) layer over the NRR electrocatalyst. Our reticular chemistry approach exploits MOF's water-repelling and molecular-concentrating effects to overcome HER-imposed bottlenecks, uncovering the unprecedented electrochemical features of NRR critical for future theoretical studies. By favoring the originally unfavored NRR, we envisage our electrocatalytic design as a starting point for high-performance nitrogen-to-ammonia electroconversion directly from water vapor-abundant air to address increasing global demand of ammonia in (bio)chemical and energy industries.

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

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

Coupling spectroscopic and chromatographic techniques for evaluation of the depositional history of hydrocarbons in a subtropical estuary

International Nuclear Information System (INIS)

Martins, César C.; Doumer, Marta E.; Gallice, Wellington C.; Dauner, Ana Lúcia L.; Cabral, Ana Caroline; Cardoso, Fernanda D.

2015-01-01

Spectroscopic and chromatographic techniques can be used together to evaluate hydrocarbon inputs to coastal environments such as the Paranaguá estuarine system (PES), located in the SW Atlantic, Brazil. Historical inputs of aliphatic hydrocarbons (AHs) and polycyclic aromatic hydrocarbons (PAHs) were analyzed using two sediment cores from the PES. The AHs were related to the presence of biogenic organic matter and degraded oil residues. The PAHs were associated with mixed sources. The highest hydrocarbon concentrations were related to oil spills, while relatively low levels could be attributed to the decrease in oil usage during the global oil crisis. The results of electron paramagnetic resonance were in agreement with the absolute AHs and PAHs concentrations measured by chromatographic techniques, while near-infrared spectroscopy results were consistent with unresolved complex mixture (UCM)/total n-alkanes ratios. These findings suggest that the use of a combination of techniques can increase the accuracy of assessment of contamination in sediments. - Highlights: • Historical inputs of hydrocarbons in a subtropical estuary were evaluated. • Spectroscopic and chromatographic methods were used in combination. • High hydrocarbon concentrations were related to anthropogenic activities. • Low hydrocarbon levels could be explained by the 1970s global oil crisis. - Spectroscopic and chromatographic techniques could be used together to evaluate hydrocarbon inputs to coastal environments

Ion chromatographic determination of Di-n-butyl phosphate in degraded organic solvent

International Nuclear Information System (INIS)

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

2011-01-01

In the present work a method for the determination of Di-n-butyl phosphate in organic streams using Ion Chromatography technique is developed and described here. The method involves the separation of Di-n-butyl phosphate (DBP) from 30% TBP-NPH (Tri-n-butylphosphate diluted in Normal Paraffin Hydrocarbon) and uranium/nitric acid matrix by an extraction of DBP in alkaline medium and subsequent ion-exchange separation in ion chromatography column followed by suppressed conductivity detection. Direct determination of DBP in lean/loaded organic solvent will lead to in accurate determination of DBP due to organic interference. DBP is quantified to lower limit of 1 ppm with 3% RSD. The results obtained with ion chromatographic technique are compared with those obtained by standard gas chromatographic technique. The developed method is much faster and total analysis can be completed within two hours. (author)

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.

Dose-modeling study to compare external beam techniques from protocol NSABP B-39/RTOG 0413 for patients with highly unfavorable cardiac anatomy

International Nuclear Information System (INIS)

Hiatt, Jessica R.; Evans, Suzanne B.; Price, Lori Lyn; Cardarelli, Gene A.; Di Petrillo, Thomas A.; Wazer, David E.

2006-01-01

Purpose: The aim of this study was to select patients with heart anatomy that is specifically unfavorable for tangential irradiation in whole-breast radiotherapy (WBRT), to be used as an experimental cohort to compare cardiac dosimetric and radiobiological parameters of three-dimensional conformal external beam accelerated partial breast irradiation (3D-CRT APBI) to WBRT with techniques as defined by the National Surgical Adjuvant Breast and Bowel Project (NSABP) B-39/Radiation Therapy Oncology Group (RTOG) 0413 clinical trial. Methods and Materials: A dosimetric modeling study that compared WBRT and 3D-CRT APBI was performed on CT planning data from 8 patients with left-sided breast cancer. Highly unfavorable cardiac anatomy was defined by the measured contact of the myocardium with the anterior chest wall in the axial and para-sagittal planes. Treatment plans of WBRT and 3D-CRT APBI were generated for each patient in accordance with NSABP B-39/RTOG 0413 protocol. Dose-volume relationships of the heart, including the V 5 min (minimum dose delivered to 5% of the cardiac volume), biological effective dose (BED) of the V 5 min, and normal tissue complication probability (NTCP) were analyzed and compared. Results: Despite expected anatomic variation, significantly large differences were found favoring 3D-CRT APBI in cumulative dose-volume histograms (p 5 min (mean difference, 24.53 Gy; p 5 min (85%, p < 0.01). Conclusions: Use of 3D-CRT APBI can demonstrate improved sparing of the heart in select patients with highly unfavorable cardiac anatomy for WBRT, and may result in reduced risk of cardiac morbidity and mortality

Biomimetic chromatographic analysis of selenium species: Application for the estimation of their pharmacokinetic properties

Energy Technology Data Exchange (ETDEWEB)

Tsopelas, Fotios [National Technical University of Athens, Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, Athens (Greece); University of Athens, Laboratory of Pharmaceutical Chemistry, School of Pharmacy, Athens (Greece); Tsantili-Kakoulidou, Anna [University of Athens, Laboratory of Pharmaceutical Chemistry, School of Pharmacy, Athens (Greece); Ochsenkuehn-Petropoulou, Maria [National Technical University of Athens, Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, Athens (Greece)

2010-07-15

The retention behavior of selenites, selenates, seleno-dl-methionine, selenocystine, selenocystamine, selenourea, dimethyl selenide, and dimethyl diselenide was investigated by means of biomimetic liquid chromatography. For this purpose, two immobilized artificial membrane (IAM) columns, namely, IAM.PC.DD2 and IAM.PC.MG, and two immobilized plasma protein columns, human serum albumin (HSA) and {alpha}{sub 1}-acid glycoprotein (AGP) columns, were employed using different mobile phase conditions in respect to pH and buffer composition. In general, satisfactory interrelations between retention factors obtained with the two IAM stationary phases and HSA/AGP columns were obtained. Large differences were observed between biomimetic retention factors and octanol-water logD values, since the latter fail to describe electrostatic interactions. In contrast, despite the column diversity, the net retention outcome on all four biomimetic columns was quite similar, especially in the presence of phosphate-buffered saline, which by its effective shielding alleviates the differences between the stationary phases. Of the two IAM columns, IAM.PC.DD2 showed better performance when compared with HSA and AGP columns as well as to octanol-water partitioning. Biomimetic chromatographic indices were further used to estimate the percentage of human oral absorption and plasma protein binding of the eight selenium species investigated, according to equations previously reported in the literature. The estimated values of human oral absorption imply moderate absorption only for dimethyl diselenide, which also may exhibit considerable plasma protein binding. Moderate affinity for plasma proteins should also be expected for dimethyl selenide and selenocystamine. (orig.)

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

Hybrid Online Labs: Making Remote Laboratories Usable Under Unfavorable Bandwidth Conditions

Directory of Open Access Journals (Sweden)

Kayode Peter Ayodele

2012-11-01

Full Text Available One of few limitations of remote laboratory technology is the fact that access and usability of such laboratories depend largely on the existence of favorable bandwidth conditions between the remote user and the system under test. This dependence is regrettable because some of the institutions likely to find remote laboratories attractive are also those most likely to have severe bandwidth limitations. Also, a typical remote laboratory will be completely unusable to remote students in the event of an outright network downtime. In this paper, we propose a hybrid online laboratory architecture that allows the automatic generation of accurate software models of remote laboratories. Such models can be hosted closer to the student and during periods of unfavorable bandwidth conditions, students can successfully interact with such models in lieu of the real hardware. We identify the challenges that need to be resolved for such a scheme to be useful and discuss the process by which suitable modeling bases were chosen. Finally we present and discuss data from a first test of the system and conclude that such a scheme holds considerable promise in changing the way remote laboratories are used and viewed.

Treatment of Early-Stage Unfavorable Hodgkin Lymphoma: Efficacy and Toxicity of 4 Versus 6 Cycles of ABVD Chemotherapy With Radiation

Energy Technology Data Exchange (ETDEWEB)

Gunther, Jillian R. [Department of Radiation Oncology, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States); Fanale, Michelle A. [Department of Lymphoma and Myeloma, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States); Reddy, Jay P. [Department of Radiation Oncology, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States); Akhtari, Mani [Department of Radiation Oncology, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States); Department of Radiation Oncology, The University of Texas Medical Branch at Galveston, Galveston, Texas (United States); Smith, Grace L.; Pinnix, Chelsea C.; Milgrom, Sarah A.; Yehia, Zeinab Abou; Allen, Pamela K.; Osborne, Eleanor M. [Department of Radiation Oncology, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States); Mawlawi, Osama [Department of Imaging Physics, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States); Dabaja, Bouthaina S., E-mail: bdabaja@mdanderson.org [Department of Radiation Oncology, The University of Texas MD Anderson Cancer Center, Houston, Texas (United States)

2016-09-01

Purpose: The German Hodgkin Study Group HD11 trial validated 4 cycles of doxorubicin, bleomycin, vinblastine, dacarbazine (ABVD) chemotherapy followed by involved field radiation therapy (IFRT) for early unfavorable Hodgkin lymphoma (HL) patients. However, practitioners often recommend 6 cycles followed by RT, especially for bulky disease. We compared patient outcomes after treatment with 4 or 6 cycles of ABVD followed by RT (IFRT and involved site RT [ISRT]). Methods and Materials: We identified 128 patients treated for early unfavorable HL (GHSG criteria) between 2000 and 2013. Clinical outcomes (overall survival [OS] and freedom from relapse [FFR]) were estimated using Kaplan-Meier analysis. Toxicities were evaluated. Results: The median follow-up time was 5.0 years. Patients received 4 (70 patients, 55%) or 6 (58 patients, 45%) cycles of chemotherapy. Bulky disease was present in 22 patients (31%; 0 stage IA, 3 stage IB, 19 stage IIA) of the 4-cycle group and 42 patients (72%; 5 stage IA, 3 stage IB, 34 stage IIA) of the 6-cycle group. For patients receiving 4 and 6 cycles, the 6-year OS was 100% and 97% (P=.35), respectively, and the 6 year FFR was 100% and 98% (P=.28), respectively. More patients received 6 cycles if they were treated before 2010 (HD11 report) (P=.01) and if they had bulky disease (P<.01). Sixty-eight percent of patients received ISRT. The 6-year FFR was 99% and 100% for patients receiving ISRT and IFRT, respectively (P=.58). More patients experienced bleomycin pulmonary toxicity in the 6-cycle group (20% vs 31%, P=.16). For patients with bulky disease, the 4-year FFR was similar with receipt of 4 (100%) or 6 (98%) cycles (P=.48) and IFRT (100%) or ISRT (98%) (P=.52). There were no deaths among patients with bulky disease. Conclusions: Patients with early unfavorable HL have excellent outcomes with 4 cycles of ABVD chemotherapy followed by ISRT. Six cycles of chemotherapy does not appear superior for disease control, even for bulky disease.

Treatment of Early-Stage Unfavorable Hodgkin Lymphoma: Efficacy and Toxicity of 4 Versus 6 Cycles of ABVD Chemotherapy With Radiation

International Nuclear Information System (INIS)

Gunther, Jillian R.; Fanale, Michelle A.; Reddy, Jay P.; Akhtari, Mani; Smith, Grace L.; Pinnix, Chelsea C.; Milgrom, Sarah A.; Yehia, Zeinab Abou; Allen, Pamela K.; Osborne, Eleanor M.; Mawlawi, Osama; Dabaja, Bouthaina S.

2016-01-01

Purpose: The German Hodgkin Study Group HD11 trial validated 4 cycles of doxorubicin, bleomycin, vinblastine, dacarbazine (ABVD) chemotherapy followed by involved field radiation therapy (IFRT) for early unfavorable Hodgkin lymphoma (HL) patients. However, practitioners often recommend 6 cycles followed by RT, especially for bulky disease. We compared patient outcomes after treatment with 4 or 6 cycles of ABVD followed by RT (IFRT and involved site RT [ISRT]). Methods and Materials: We identified 128 patients treated for early unfavorable HL (GHSG criteria) between 2000 and 2013. Clinical outcomes (overall survival [OS] and freedom from relapse [FFR]) were estimated using Kaplan-Meier analysis. Toxicities were evaluated. Results: The median follow-up time was 5.0 years. Patients received 4 (70 patients, 55%) or 6 (58 patients, 45%) cycles of chemotherapy. Bulky disease was present in 22 patients (31%; 0 stage IA, 3 stage IB, 19 stage IIA) of the 4-cycle group and 42 patients (72%; 5 stage IA, 3 stage IB, 34 stage IIA) of the 6-cycle group. For patients receiving 4 and 6 cycles, the 6-year OS was 100% and 97% (P=.35), respectively, and the 6 year FFR was 100% and 98% (P=.28), respectively. More patients received 6 cycles if they were treated before 2010 (HD11 report) (P=.01) and if they had bulky disease (P<.01). Sixty-eight percent of patients received ISRT. The 6-year FFR was 99% and 100% for patients receiving ISRT and IFRT, respectively (P=.58). More patients experienced bleomycin pulmonary toxicity in the 6-cycle group (20% vs 31%, P=.16). For patients with bulky disease, the 4-year FFR was similar with receipt of 4 (100%) or 6 (98%) cycles (P=.48) and IFRT (100%) or ISRT (98%) (P=.52). There were no deaths among patients with bulky disease. Conclusions: Patients with early unfavorable HL have excellent outcomes with 4 cycles of ABVD chemotherapy followed by ISRT. Six cycles of chemotherapy does not appear superior for disease control, even for bulky disease.

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)

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.

Advanced hyphenated chromatographic-mass spectrometry in mycotoxin determination: current status and prospects.

Science.gov (United States)

Li, Peiwu; Zhang, Zhaowei; Hu, Xiaofeng; Zhang, Qi

2013-01-01

Mass spectrometric techniques are essential for advanced research in food safety and environmental monitoring. These fields are important for securing the health of humans and animals, and for ensuring environmental security. Mycotoxins, toxic secondary metabolites of filamentous fungi, are major contaminants of agricultural products, food and feed, biological samples, and the environment as a whole. Mycotoxins can cause cancers, nephritic and hepatic diseases, various hemorrhagic syndromes, and immune and neurological disorders. Mycotoxin-contaminated food and feed can provoke trade conflicts, resulting in massive economic losses. Risk assessment of mycotoxin contamination for humans and animals generally depends on clear identification and reliable quantitation in diversified matrices. Pioneering work on mycotoxin quantitation using mass spectrometry (MS) was performed in the early 1970s. Now, unambiguous confirmation and quantitation of mycotoxins can be readily achieved with a variety hyphenated techniques that combine chromatographic separation with MS, including liquid chromatography (LC) or gas chromatography (GC). With the advent of atmospheric pressure ionization, LC-MS has become a routine technique. Recently, the co-occurrence of multiple mycotoxins in the same sample has drawn an increasing amount of attention. Thus, modern analyses must be able to detect and quantitate multiple mycotoxins in a single run. Improvements in tandem MS techniques have been made to achieve this purpose. This review describes the advanced research that has been done regarding mycotoxin determination using hyphenated chromatographic-MS techniques, but is not a full-circle survey of all the literature published on this topic. The present work provides an overview of the various hyphenated chromatographic-MS-based strategies that have been applied to mycotoxin analysis, with a focus on recent developments. The use of chromatographic-MS to measure levels of mycotoxins, including

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.)

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....

A chromatographic objective function to characterise chromatograms with unknown compounds or without standards available.

Science.gov (United States)

Alvarez-Segura, T; Gómez-Díaz, A; Ortiz-Bolsico, C; Torres-Lapasió, J R; García-Alvarez-Coque, M C

2015-08-28

Getting useful chemical information from samples containing many compounds is still a challenge to analysts in liquid chromatography. The highest complexity corresponds to samples for which there is no prior knowledge about their chemical composition. Computer-based methodologies are currently considered as the most efficient tools to optimise the chromatographic resolution, and further finding the optimal separation conditions. However, most chromatographic objective functions (COFs) described in the literature to measure the resolution are based on mathematical models fitted with the information obtained from standards, and cannot be applied to samples with unknown compounds. In this work, a new COF based on the automatic measurement of the protruding part of the chromatographic peaks (or peak prominences) that indicates the number of perceptible peaks and global resolution, without the need of standards, is developed. The proposed COF was found satisfactory with regard to the peak purity criterion when applied to artificial peaks and simulated chromatograms of mixtures built using the information of standards. The approach was applied to mixtures of drugs containing unknown impurities and degradation products and to extracts of medicinal herbs, eluted with acetonitrile-water mixtures using isocratic and gradient elution. Copyright © 2015 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

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

Gas chromatographic isolation technique for compound-specific radiocarbon analysis

International Nuclear Information System (INIS)

Uchida, M.; Kumamoto, Y.; Shibata, Y.; Yoneda, M.; Morita, M.; Kawamura, K.

2002-01-01

Full text: We present here a gas chromatographic isolation technique for the compound-specific radiocarbon analysis of biomarkers from the marine sediments. The biomarkers of fatty acids, hydrocarbon and sterols were isolated with enough amount for radiocarbon analysis using a preparative capillary gas chromatograph (PCGC) system. The PCGC systems used here is composed of an HP 6890 GC with FID, a cooled injection system (CIS, Gerstel, Germany), a zero-dead-volume effluent splitter, and a cryogenic preparative collection device (PFC, Gerstel). For AMS analysis, we need to separate and recover sufficient quantity of target individual compounds (>50 μgC). Yields of target compounds from C 14 n-alkanes to C 40 to C 30 n-alkanes and approximately that of 80% for higher molecular weights compounds more than C 30 n-alkanes. Compound specific radiocarbon analysis of organic compounds, as well as compound-specific stable isotope analysis, provide valuable information on the origins and carbon cycling in marine system. Above PCGC conditions, we applied compound-specific radiocarbon analysis to the marine sediments from western north Pacific, which showed the possibility of a useful chronology tool for estimating the age of sediment using organic matter in paleoceanographic study, in the area where enough amounts of planktonic foraminifera for radiocarbon analysis by accelerator mass spectrometry (AMS) are difficult to obtain due to dissolution of calcium carbonate. (author)

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

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.

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.

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.

ADAPTATION TO UNFAVORABLE CONDITIONS OF GROWTH: PATHOGENICITY OF ACHOLEPLASMA LAIDLAWII PG8

Directory of Open Access Journals (Sweden)

Maxim V. Trushin

2006-11-01

Full Text Available ABSTRACT:As a result of cultivation of A. laidlawii PG8 cells on the deficient medium during 480 days, the mycoplasma culture adapted in vitro to unfavorable growth conditions was obtained. The culture consisted of cells with sizes less than 0.2 µm and features of A. laidlawii PG8 ultramicroforms, nanocells. A. laidlawii PG8 culture adapted in vitro to unfavorable growth conditions shows more evident phytopathogenicity than the unadapted one. Infecting plants V. minor L. by A. laidlawii PG8 culture adapted in vitro to UGC resulted in the appearance of chloroses in 75%, necrosis – 50%, leaves marcescence – 50% and abnormalities of bine development in 30% of plants through 12 days, while infecting plants by A. laidlawii PG8 culture unadapted to UGC led to respective signs in 40%, 25%, 25% and 0% of samples, respectively, through 30 days. The ability of A. laidlawii PG8 to form UMF resistant to stress factors in UGC with high phytopathogenic potential seems to demand a new approach to investigate the precise mechanisms of interacting the mycoplasma with host organisms.RESUMENComo resultado del cultivo de células de A. laidlawii PG8 en medio deficiente durante 480 días, fue obtenido un cultivo de mycoplasma adaptado in vitro a las condiciones desfavorables del crecimiento. El cultivo consistió en células con tamaño menor de 0.2 µm y características PG8 ultramicroformas de A. laidlawii nanocélulas. El cultivo de A. laidlawii PG8 adaptado in vitro a condiciones desfavorables del crecimiento muestra más evidente fitopatogenicidad que el inadaptado. Plantas infectadas V. minor L. por el cultivo del A. laidlawii PG8 adaptado in vitro a UGC dio como resultado la aparición de clorosis en el 75%, necrosis en el 50%, marcescencia de las hojas en el 50% y anormalidades del desarrollo del bine en el 30% de plantas a los 12 días, mientras que las plantas infectadas por el cultivo del A. laidlawii PG8 inadaptado a UGC, condujo a dichos signos en

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

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

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

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.

Dose escalation using conformal high-dose-rate brachytherapy improves outcome in unfavorable prostate cancer

International Nuclear Information System (INIS)

Martinez, Alvaro A.; Gustafson, Gary; Gonzalez, Jose; Armour, Elwood; Mitchell, Chris; Edmundson, Gregory; Spencer, William; Stromberg, Jannifer; Huang, Raywin; Vicini, Frank

2002-01-01

Purpose: To overcome radioresistance for patients with unfavorable prostate cancer, a prospective trial of pelvic external beam irradiation (EBRT) interdigitated with dose-escalating conformal high-dose-rate (HDR) prostate brachytherapy was performed. Methods and Materials: Between November 1991 and August 2000, 207 patients were treated with 46 Gy pelvic EBRT and increasing HDR brachytherapy boost doses (5.50-11.5 Gy/fraction) during 5 weeks. The eligibility criteria were pretreatment prostate-specific antigen level ≥10.0 ng/mL, Gleason score ≥7, or clinical Stage T2b or higher. Patients were divided into 2 dose levels, low-dose biologically effective dose 93 Gy (149 patients). No patient received hormones. We used the American Society for Therapeutic Radiology and Oncology definition for biochemical failure. Results: The median age was 69 years. The mean follow-up for the group was 4.4 years, and for the low and high-dose levels, it was 7.0 and 3.4 years, respectively. The actuarial 5-year biochemical control rate was 74%, and the overall, cause-specific, and disease-free survival rate was 92%, 98%, and 68%, respectively. The 5-year biochemical control rate for the low-dose group was 52%; the rate for the high-dose group was 87% (p<0.001). Improvement occurred in the cause-specific survival in favor of the brachytherapy high-dose level (p=0.014). On multivariate analysis, a low-dose level, higher Gleason score, and higher nadir value were associated with increased biochemical failure. The Radiation Therapy Oncology Group Grade 3 gastrointestinal/genitourinary complications ranged from 0.5% to 9%. The actuarial 5-year impotency rate was 51%. Conclusion: Pelvic EBRT interdigitated with transrectal ultrasound-guided real-time conformal HDR prostate brachytherapy boost is both a precise dose delivery system and a very effective treatment for unfavorable prostate cancer. We demonstrated an incremental beneficial effect on biochemical control and cause

[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 separation of fructose from date syrup.

Science.gov (United States)

Al Eid, Salah M

2006-01-01

The objective of this study is to provide a process for separating fructose from a mixture of sugars containing essentially fructose and glucose, obtained from date palm fruits. The extraction procedure of date syrup from fresh dates gave a yield of 86.5% solids after vacuum drying. A process for separating fructose from an aqueous solution of date syrup involved adding the date syrup solutions (20, 30 and 40% by weight) to a chromatographic column filled with Dowex polystyrene strong cation exchange gel matrix resin Ca2 + and divinylbenzene, a functional group, sulfonic acid, particle size 320 microm, with a flow rate of 0.025 and 0.05 bed volume/min, under 30 and 70 degrees C column temperature. After the date sugar solution batch, a calculated quantity of water was added to the column. Glucose was retained by the resin more weakly than fructose and proceeded faster into the water batch flowing ahead. Three fractions were collected: a glucose-rich fraction, a return fraction, and a fructose-rich fraction. The return fraction is based on when the peaks of fructose and glucose were reached, which could be determined by means of an analyzer (polarimeter) based on the property of glucose and fructose solutions to turn the polarization level of polarized light. A high yield of fructose is obtained at 70 degrees C column temperature with a flow rate of 0.025 bed volume/min and date syrup solution containing 40% sugar concentration. The low recovery by weight obtained using date syrup solutions having a sugar concentration of 20 and 30%, encourages the use of a concentration of 40%. However, with the 40% date syrup supply the average concentrations of glucose and fructose in the return fractions were more than 40%, which can be used for diluting the thick date syrup solution extracted from dates.

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.

A Binomial Modeling Approach for Upscaling Colloid Transport Under Unfavorable Attachment Conditions: Emergent Prediction of Nonmonotonic Retention Profiles

Science.gov (United States)

Hilpert, Markus; Johnson, William P.

2018-01-01

We used a recently developed simple mathematical network model to upscale pore-scale colloid transport information determined under unfavorable attachment conditions. Classical log-linear and nonmonotonic retention profiles, both well-reported under favorable and unfavorable attachment conditions, respectively, emerged from our upscaling. The primary attribute of the network is colloid transfer between bulk pore fluid, the near-surface fluid domain (NSFD), and attachment (treated as irreversible). The network model accounts for colloid transfer to the NSFD of downgradient grains and for reentrainment to bulk pore fluid via diffusion or via expulsion at rear flow stagnation zones (RFSZs). The model describes colloid transport by a sequence of random trials in a one-dimensional (1-D) network of Happel cells, which contain a grain and a pore. Using combinatorial analysis that capitalizes on the binomial coefficient, we derived from the pore-scale information the theoretical residence time distribution of colloids in the network. The transition from log-linear to nonmonotonic retention profiles occurs when the conditions underlying classical filtration theory are not fulfilled, i.e., when an NSFD colloid population is maintained. Then, nonmonotonic retention profiles result potentially both for attached and NSFD colloids. The concentration maxima shift downgradient depending on specific parameter choice. The concentration maxima were also shown to shift downgradient temporally (with continued elution) under conditions where attachment is negligible, explaining experimentally observed downgradient transport of retained concentration maxima of adhesion-deficient bacteria. For the case of zero reentrainment, we develop closed-form, analytical expressions for the shape, and the maximum of the colloid retention profile.

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.)

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

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.

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

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.

A validated calculator to estimate risk of cesarean after an induction of labor with an unfavorable cervix.

Science.gov (United States)

Levine, Lisa D; Downes, Katheryne L; Parry, Samuel; Elovitz, Michal A; Sammel, Mary D; Srinivas, Sindhu K

2018-02-01

Induction of labor occurs in >20% of pregnancies, which equates to approximately 1 million women undergoing an induction in the United States annually. Regardless of how common inductions are, our ability to predict induction success is limited. Although multiple risk factors for a failed induction have been identified, risk factors alone are not enough to quantify an actual risk of cesarean for an individual woman undergoing a cesarean. The objective of this study was to derive and validate a prediction model for cesarean after induction with an unfavorable cervix and to create a Web-based calculator to assist in patient counseling. Derivation and validation of a prediction model for cesarean delivery after induction was performed as part of a planned secondary analysis of a large randomized trial. A predictive model for cesarean delivery was derived using multivariable logistic regression from a large randomized trial on induction methods (n = 491) that took place from 2013 through 2015 at an academic institution. Full-term (≥37 weeks) women carrying a singleton gestation with intact membranes and an unfavorable cervix (Bishop score ≤6 and dilation ≤2 cm) undergoing an induction were included in this trial. Both nulliparous and multiparous women were included. Women with a prior cesarean were excluded. Refinement of the prediction model was performed using an observational cohort of women from the same institution who underwent an induction (n = 364) during the trial period. An external validation was performed utilizing a publicly available database (Consortium for Safe Labor) that includes information for >200,000 deliveries from 19 hospitals across the United States from 2002 through 2008. After applying the same inclusion and exclusion criteria utilized in the derivation cohort, a total of 8466 women remained for analysis. The discriminative power of each model was assessed using a bootstrap, bias-corrected area under the curve. The cesarean delivery

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

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.

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.

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

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.

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.

Inorganic ion-exchangers. Their role in chromatographic radionuclide generators for the decade 1993-2002

International Nuclear Information System (INIS)

Mushtaq, A.

2004-01-01

Ion-exchangers are found not only in water purification processes, the original major application, but also in analytical chemistry for the separation and isolation of elements, hydrometallurgy, inorganic chemistry and biochemistry, in food technology, and of course in many specialized fields related to the utilization of atomic energy. The use of organic ion-exchangers is limited by virtue of their limited stability under harsh conditions, whereas inorganic ion-exchangers possess important properties, which make them very useful for chemical separation and purification in intense radiation fields. The availability of short-lived radionuclides from radionuclide generators provides an inexpensive and convenient alternative to in-house radioisotope production facilities such as accelerators and cyclotrons. Due to their simplicity of operation, chromatographic based generators have been the method of choice, although generators based on solvent extraction and on volatilization and sublimation have also been developed, and are routinely used. In this paper use of inorganic ion-exchangers for the development of radionuclide generators for the decade 1993-2002 has been compiled. (author)

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.

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

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

Elevated NT-proBNP is associated with unfavorably altered plasma fibrin clot properties in atrial fibrillation.

Science.gov (United States)

Matusik, Paweł T; Matusik, Patrycja S; Kornacewicz-Jach, Zdzisława; Małecka, Barbara; Ząbek, Andrzej; Undas, Anetta

2017-09-15

Dense fibrin clot formation and hypofibrinolysis have been reported in atrial fibrillation (AF). It is unclear which factors affect fibrin clot properties in AF. We investigated plasma fibrin clot permeability (K s ), clot lysis time (CLT), endogenous thrombin potential (ETP) as well as other coagulation and fibrinolysis parameters along with N-terminal pro-B-type natriuretic peptide (NT-proBNP) in 160 AF patients (median age, 70.5years). Previous stroke (n=15; 9.4%) was associated with decreased K s (P=0.04) and longer CLT (P=0.005), together with higher antiplasmin (P=0.03) and lower tissue-type plasminogen activator (P=0.01). Lower K s (P=0.04) and tendency towards longer CLT (P=0.10) were observed in patients with a left atrium diameter>40mm. Patients with a CHA 2 DS 2 -VASc score of 3 or more (82.5%) were characterized by higher thrombin-activatable fibrinolysis inhibitor antigen (P=0.009). K s was inversely correlated with log NT-proBNP (r=-0.34, PCLT was positively correlated with log NT-proBNP (R=0.61, PCLT (the top quartile,≥109min). In AF patients prothrombotic fibrin clot properties assessed ex vivo are determined by PAI-1 and NT-proBNP and this phenotype is associated with prior ischemic stroke. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Synthesis of chromatographic standards and establishment of a method for the quantification of the fatty ester composition of biodiesel from babassu oil

International Nuclear Information System (INIS)

Urioste, Daniele; Castro, Matheus B.A.; Biaggio, Francisco C.; Castro, Heizir F. de

2008-01-01

Several alkyl esters were synthesized, purified, characterized by 1 H NMR and employed as standards for establishing chromatographic methods to monitor their formation in the synthesis of biodiesel. The efficiency of the chromatographic methods was confirmed with the products of enzymatic transesterification of babassu oil with different alcohols (C 2 to C 4 ), using Lipozyme as catalyst. (author)

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.

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

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)

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.

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

ACE DD genotype is unfavorable to Korean short-term muscle power athletes.

Science.gov (United States)

Kim, C-H; Cho, J-Y; Jeon, J Y; Koh, Y G; Kim, Y-M; Kim, H-J; Park, M; Um, H-S; Kim, C

2010-01-01

The purpose of this study was to test the hypothesis that the ACE DD genotype is unfavorably associated with the ultimate power-oriented performance. To test the hypothesis we recruited a total of 848 subjects including 55 international level power-oriented athletes (High-performance), 100 national level power-oriented athletes (Mid-performance) and 693 healthy controls (Control) in Korea. Then the distributions of ACE polymorphism throughout these groups were analyzed. As a result, there was a gradual decrease of frequencies of the DD genotype with advancing levels of performance (Control vs. Mid-performance vs. High-performance=17.2% vs. 10.0% vs. 5.5%, p=0.002). Also, the frequencies of D allele decreased gradually with advancing levels of performance (Control vs. Mid-performance vs. High-performance=42.6% vs. 35.0% vs. 30.9%, pDD genotype and the D allele. This finding gave 3.83 times lower probability of success in power-oriented sports for individuals with the DD genotype than those with the II+ ID genotype. In conclusion, these results indicate that Korean power-oriented athletes with a lower frequency of the DD genotype had a lower probability of success in power-oriented sports. Georg Thieme Verlag KG Stuttgart, New York.

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)

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)

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.

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)

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...

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.

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)

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...

Attenuated associations between increasing BMI and unfavorable lipid profiles in Chinese Buddhist vegetarians.

Science.gov (United States)

Zhang, Hui-Jie; Han, Peng; Sun, Su-Yun; Wang, Li-Ying; Yan, Bing; Zhang, Jin-Hua; Zhang, Wei; Yang, Shu-Yu; Li, Xue-Jun

2013-01-01

Obesity is related to hyperlipidemia and risk of cardiovascular disease. Health benefits of vegetarian diets have well-documented in the Western countries where both obesity and hyperlipidemia were prevalent. We studied the association between BMI and various lipid/lipoprotein measures, as well as between BMI and predicted coronary heart disease probability in lean, low risk populations in Southern China. The study included 170 Buddhist monks (vegetarians) and 126 omnivore men. Interaction between BMI and vegetarian status was tested in the multivariable regression analysis adjusting for age, education, smoking, alcohol drinking, and physical activity. Compared with omnivores, vegetarians had significantly lower mean BMI, blood pressures, total cholesterol, low density lipoprotein cholesterol, high density lipoprotein cholesterol, total cholesterol to high density lipoprotein ratio, triglycerides, apolipoprotein B and A-I, as well as lower predicted probability of coronary heart disease. Higher BMI was associated with unfavorable lipid/lipoprotein profile and predicted probability of coronary heart disease in both vegetarians and omnivores. However, the associations were significantly diminished in Buddhist vegetarians. Vegetarian diets not only lower BMI, but also attenuate the BMI-related increases of atherogenic lipid/ lipoprotein and the probability of coronary heart disease.

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...

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)

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.

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

Determination of biologically active phenols and polyphenols in various objects by chromatographic techniques

International Nuclear Information System (INIS)

Kochetova, M V; Semenistaya, E N; Larionov, Oleg G; Revina, A A

2007-01-01

Chromatographic techniques for determination of biologically active phenols and polyphenols are considered. Various methods for sample preparation and detection are compared. The advantages of high performance liquid chromatography with spectrophotometric detection for determination of antioxidants are demonstrated. Data on determination of biologically active phenols and polyphenols published in the period from 1995 to 2005 are analysed.

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...

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)

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.

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.

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

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.

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

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)

Restoration of unfavorably positioned implants for a partially endentulous patient by using an overdenture retained with a milled bar and attachments: a clinical report.

Science.gov (United States)

Asvanund, Chanavut; Morgano, Steven M

2004-01-01

The restorative dentist may encounter patients with previously placed misaligned implants that are well integrated. Often, these patients have deficient alveolar ridge contour further complicating treatment options. This clinical report describes a treatment approach for a partially edentulous patient with unfavorably positioned implants that incorporated: (1) an implant-supported milled bar with a removable, metal-acrylic resin, partial overdenture, (2) implant-supported single crowns, and (3) crowns retained by natural teeth.

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 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.

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.

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.

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.

Body fat percentage is better than indicators of weight status to identify children and adolescents with unfavorable lipid profile.

Science.gov (United States)

Oliosa, Polyana Romano; Zaniqueli, Divanei; Alvim, Rafael de Oliveira; Barbosa, Miriam Carmo Rodrigues; Mill, José Geraldo

2018-01-05

To assess whether the indicators of weight status body mass index and waist-to-height ratio are similar to body fat percentage to identify obese children and adolescents with unfavorable lipid profile. This was a cross-sectional study involving 840 children and adolescents (6-18 years). The same individuals were classified as non-obese (

unfavorable lipid profile, mainly among girls. Copyright © 2017. Published by Elsevier Editora Ltda.

Effect of Iron and Magnesium on Alloy AL9M Structure and Properties

Science.gov (United States)

Bazhenov, V. E.; Koltygin, A. V.; Belov, V. D.

2017-09-01

The effect of iron impurity on the structure and properties of aluminum alloy AL9M, especially its action on magnesium distribution within the structure, is studied. The microstructure of a cast component of this alloy broken during operation is analyzed. It is shown that iron impurity has an unfavorable effect on structure and mechanical properties of a casting due to appearance of Al9Fe2Si and Al18Fe2Mg7Si10 intermetallics. Formation of these intermetallics consumes a considerable amount of magnesium and lowers the content of the Q(Al5Cu2Mg8Si6) strengthening phase in the alloy structure.

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

Chromatographic Techniques for Rare Earth Elements Analysis

Science.gov (United States)

Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

2017-04-01

The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

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

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.

Chromatographic properties PLOT multicapillary columns.

Science.gov (United States)

Nikolaeva, O A; Patrushev, Y V; Sidelnikov, V N

2017-03-10

Multicapillary columns (MCCs) for gas chromatography make it possible to perform high-speed analysis of the mixtures of gaseous and volatile substances at a relatively large amount of the loaded sample. The study was performed using PLOT MCCs for gas-solid chromatography (GSC) with different stationary phases (SP) based on alumina, silica and poly-(1-trimethylsilyl-1-propyne) (PTMSP) polymer as well as porous polymers divinylbenzene-styrene (DVB-St), divinylbenzene-vinylimidazole (DVB-VIm) and divinylbenzene-ethylene glycol dimethacrylate (DVB-EGD). These MCCs have the efficiency of 4000-10000 theoretical plates per meter (TP/m) and at a column length of 25-30cm can separate within 10-20s multicomponent mixtures of substances belonging to different classes of chemical compounds. The sample amount not overloading the column is 0.03-1μg and depends on the features of a porous layer. Examples of separations on some of the studied columns are considered. Copyright © 2017 Elsevier B.V. All rights reserved.

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.)

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...

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.

Chromatographic techniques used in the laboratory scale fractionation and purification of plasma

International Nuclear Information System (INIS)

Siti Najila Mohd Janib; Wan Hamirul Bahrin Wan Kamal; Shaharuddin Mohd

2004-01-01

Chromatography is a powerful technique used in the separation as well as purification of proteins for use as biopharmaceuticals or medicines. Scientists use many different chromatographic techniques in biotechnology as they bring a molecule from its initial identification stage to the stage of it becoming a marketed product. The most commonly used of these techniques is liquid chromatography (1,C). This technique can be used to separate the target molecule from undesired contaminants, as well as to analyse the final product for the requisite purity as established by governmental regulatory groups such as the FDA. Some examples of LC techniques include: ion exchange (IEC), hydrophobic interaction (HIC), gel filtration (GF), affinity (AC) and reverse phase (RPC) chromatography. These techniques are very versatile and can be used at any stage of the purification process i.e. capture, intermediate purification phase and polishing. The choice of a particular technique is dependent upon the nature of the target protein as well as its intended final use. This paper describes the preliminary work done on the chromatographic purification of factor VIII (FVIII), factor IX (FIX), albumin and IgG from plasma. Results, in particular, in the isolation of albumin and IgG using IEC, have been promising. Preparation and production of cryoprecipitate to yield FVIII and FIX have also been successful. (Author)

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…

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%.

Sorption and chromatographic techniques for processing liquid waste of nuclear fuel cycle

International Nuclear Information System (INIS)

Gelis, V.M.; Milyutin, V.V.; Chuveleva, E.A.; Maslova, G.B.; Kudryavtseva, S.P.; Firsova, L.A.; Kozlitin, E.A.

2000-01-01

In the spent nuclear fuel processing procedures the significant quantity of high level liquid waste containing long-lived high toxic radionuclides of cesium, strontium, promethium, americium, curium, etc. is generated. Separation of those radionuclides from the waste not merely simplifies the further safe waste handling but also reduces the waste processing operation costs due to the market value of certain individual radionuclide preparations. Recovery and separation of high grade pure long-lived radionuclide preparations is frequently performed by means of chromatographic techniques. (authors)

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

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.

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)

The effect of quitting smoking on the risk of unfavorable events after surgical treatment of oral potentially malignant lesions

DEFF Research Database (Denmark)

Vladimirov, B S; Schiødt, Morten

2009-01-01

smokers at the time of diagnosis and were treated surgically. Patients were advised to quit smoking at each visit. The change of smoking habits and occurrence of unfavorable events were noted during follow-up. Descriptive statistics, Fischer's exact test, Kaplan-Meier curves with log-rank test, and Cox......The aim of this study was to examine if cessation of smoking after surgical excision of oral potentially malignant lesions in smokers reduced the risk of recurrences, development of new lesions or malignancies. 51 patients with oral leukoplakia or erythroplakia were included. They were daily...... proportional hazards model were used for analysis. 16 patients (31%) quit smoking during the observation period. Only one quitter (6%) developed recurrence compared with 11 continuing smokers (33%) (p

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.

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

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.

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

The role of multiploidy as unfavorable prognostic variable in colorectal cancer.

Science.gov (United States)

Cosimelli, M; D'Agnano, I; Tedesco, M; D'Angelo, C; Botti, C; Giannarelli, D; Vasselli, S; Cavaliere, F; Zupi, G; Cavaliere, R

1998-01-01

To analyze the prognostic value of DNA multiploidy in a prospective study on frozen surgical tissue samples from primary colorectal cancer. Survival data from eleven prospective studies collectively comprising about thirteen hundred patients showed that aneuploidy correlated with a 5-year disease-free survival (DFS) significantly poorer than diploidy, and showed the limited prognostic value of results from retrospective studies employing paraffin-embedded material. Multiple tumor samples of fresh/frozen surgical tissues from 120 colorectal cancer patients who had undergone radical surgery were taken for flow cytometric analysis of DNA content, and proliferative activity, shown as percentage of cells in S-phase (%S). The minimum follow-up of this series was 30 months. Univariate and multivariate analyses determined the independent significance of both clinical and biological variable on DFS. Values of %S equal to or higher than 17.3 correlated with a 5-year DFS poorer than values lower than 17.3 (44.5% vs 85.2% respectively; p = .03), even if only in patients younger than 64. The subgroup with multiploid tumors showed a significantly poorer 5-year DFS (44.5% vs. 62.6% in the non multiploid patients; p = .02). Subgrouping the Dukes'B stage alone by multiploidy, the difference in DFS was much more evident (31.2% vs. 68% respectively; p = .0004) and multivariate analysis showed multiploidy as the only significant variable. Above all, adjuvant therapy did not absolutely modify the unfavorable outcome of the multiploid Dukes'B patients. The prospective evaluation of ploidy allowed us to identify a very high-risk subgroup of patients with multiploid tumors. This biological characterization was easy to demonstrate and, above all in node-negative patients, reliable and very effective in terms of prognosis. The presence of multiploidy should result in a more aggressive therapeutic approach in the adjuvant setting.

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

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.

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.

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.

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.

Coronary fluorine-18-sodium fluoride uptake is increased in healthy adults with an unfavorable cardiovascular risk profile

DEFF Research Database (Denmark)

Blomberg, Björn A; Thomassen, Anders; de Jong, Pim A

2017-01-01

OBJECTIVE: Coronary artery fluorine-18-sodium fluoride (F-NaF) uptake reflects coronary artery calcification metabolism and is considered to be an early prognostic marker of coronary heart disease. This study evaluated the relationship between coronary artery F-NaF uptake and cardiovascular risk ...... adults at low cardiovascular risk and that an unfavorable cardiovascular risk profile is associated with a marked increase in coronary artery F-NaF uptake.......OBJECTIVE: Coronary artery fluorine-18-sodium fluoride (F-NaF) uptake reflects coronary artery calcification metabolism and is considered to be an early prognostic marker of coronary heart disease. This study evaluated the relationship between coronary artery F-NaF uptake and cardiovascular risk...... in healthy adults at low cardiovascular risk. PARTICIPANTS AND METHODS: Study participants underwent blood pressure measurements, blood analyses, and coronary artery F-NaF PET/CT imaging. In addition, the 10-year risk for the development of cardiovascular disease, on the basis of the Framingham Risk Score...

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.

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.

Enhancing the Properties of Carbon and Gold Substrates by Surface Modification

Energy Technology Data Exchange (ETDEWEB)

Harnisch, Jennifer Anne [Iowa State Univ., Ames, IA (United States)

2001-01-01

The properties of both carbon and gold substrates are easily affected by the judicious choice of a surface modification protocol. Several such processes for altering surface composition have been published in literature. The research presented in this thesis primarily focuses on the development of on-column methods to modify carbon stationary phases used in electrochemically modulated liquid chromatography (EMLC). To this end, both porous graphitic carbon (PGC) and glassy carbon (GC) particles have been modified on-column by the electroreduction of arenediazonium salts and the oxidation of arylacetate anions (the Kolbe reaction). Once modified, the carbon stationary phases show enhanced chromatographic performance both in conventional liquid chromatographic columns and EMLC columns. Additionally, one may also exploit the creation of aryl films to by electroreduction of arenediazonium salts in the creation of nanostructured materials. The formation of mercaptobenzene film on the surface of a GC electrode provides a linking platform for the chemisorption of gold nanoparticles. After deposition of nanoparticles, the surface chemistry of the gold can be further altered by self-assembled monolayer (SAM) formation via the chemisorption of a second thiol species. Finally, the properties of gold films can be altered such that they display carbon-like behavior through the formation of benzenehexathiol (BHT) SAMs. BHT chemisorbs to the gold surface in a previously unprecedented planar fashion. Carbon and gold substrates can be chemically altered by several methodologies resulting in new surface properties. The development of modification protocols and their application in the analytical arena is considered herein.

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

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.

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.

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.

D meson production asymmetry, unfavored fragmentation, and consequences for prompt atmospheric neutrino production

Science.gov (United States)

Maciuła, Rafał; Szczurek, Antoni

2018-04-01

We consider unfavored light quark/antiquark to D meson fragmentation. We discuss nonperturbative effects for small transverse momenta. The asymmetry for D+ and D- production measured by the LHCb collaboration provides natural constraints on the parton (quark/antiquark) fragmentation functions. We find that already a fraction of q /q ¯→D fragmentation probability is sufficient to account for the measured asymmetry. We make predictions for similar asymmetry for neutral D mesons. Large D -meson production asymmetries are found for large xF which is related to dominance of light quark/antiquark q /q ¯→D fragmentation over the standard c →D fragmentation. As a consequence, prompt atmospheric neutrino flux at high neutrino energies can be much larger than for the conventional c →D fragmentation. The latter can constitute a sizeable background for the cosmic neutrinos claimed to be observed recently by the IceCube Observatory. Large rapidity-dependent D+/D- and D0/D¯0 asymmetries are predicted for low (√{s }=20 - 100 GeV ) energies. The q /q ¯→D fragmentation leads to enhanced production of D mesons at low energies. At √{s }=20 GeV the enhancement factor with respect to the conventional contribution is larger than a factor of five. In the considered picture the large-xF D mesons are produced dominantly via fragmentation of light quarks/antiquarks. Predictions for fixed target p + 4He collisions relevant for a fixed target LHCb experiment are presented.

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.

Effect of kinetic properties of extraction systems on separation of some elements by liquid chromatography method with free fixed phase

International Nuclear Information System (INIS)

Fedotov, P.S.; Maryutina, T.A.; Pichugin, A.A.; Spivakov, B.Ya.

1993-01-01

Effect of kinetic properties of a series of extraction systems on the separation of certain elements by the method of liquid chromatography with free fixed phase is considered. Chromatographic behaviour of europium 3 and iron 3 ions when using systems based on di-2-ethylhexylphosphovers acid and tetraphenylmethylenediphosphine dioxide is investigated. Kinetic properties of the extraction systems used are studied by diffusion cell method with mixing, europium 3 and iron 3 mass transfer coefficients are determined

The adaptive internet application for interpretation of the transformer oil gas chromatographic analysis results

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Polužanski Vladimir

2015-01-01

Full Text Available This paper describes an adaptive Internet application for the interpretation of the transformer oil gas chromatographic analysis results. The first version of the application is developed by following an evolutionary software development concept. The most important software development risks and the appropriate solutions are described. An open-source web framework named Bootstrap is used for an application implementation. The application is developed by using ASP.NET and MS SQL server.

The counterintuitive role of extra-column volume in the determination of column efficiency and scaling of chromatographic processes

NARCIS (Netherlands)

Schultze-Jena, A.; Boon, M.A.; Bussmann, P.J.Th.; Janssen, A.E.M.; Padt, van der A.

2017-01-01

In industrial liquid separation processes chromatography often has a key function in the optimization of yield and purity. For the design of an industrial system, chromatographic processes are generally simulated using mathematical models, tested and optimized at laboratory level, and then scaled

The counterintuitive role of extra-column volume in the determination of column efficiency and scaling of chromatographic processes

NARCIS (Netherlands)

Schultze-Jena, A.; Boon, M.A.; Bussmann, P.J.T.; Janssen, A.E.M.; Padt, A. van der

2017-01-01

In industrial liquid separation processes chromatography often has a key function in the optimization of yield and purity. For the design of an industrial system, chromatographic processes are generally simulated using mathematical models, tested and optimized at laboratory level, and then scaled up

HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC PROFILING OF TRYPTOPHAN AND RELATED INDOLES IN BODY-FLUIDS AND TISSUES OF CARCINOID PATIENTS

NARCIS (Netherlands)

KEMA, IP; SCHELLINGS, AMJ; HOPPENBROUWERS, CJM; RUTGERS, HM; DEVRIES, EGE; MUSKIET, FAJ

1993-01-01

A high performance liquid chromatographic method with quaternary gradient elution and fluorometric detection was developed for profiling of tryptophan (TRP), 5-hydroxytryptophan, serotonin (5-HT) and 5-hydroxyindole-3-acetic acid (5-HIAA) in urine, platelet-rich plasma and (tumour) tissue of

Origins of the Unfavorable Activation and Reaction Energies of 1-Azadiene Heterocycles Compared to 2-Azadiene Heterocycles in Diels-Alder Reactions.

Science.gov (United States)

Fell, Jason S; Martin, Blanton N; Houk, K N

2017-02-17

The reactivities of butadiene, cyclopentadiene, furan, thiophene, pyrrole, and their 1-aza- and 2-aza-derivatives in Diels-Alder reactions with ethylene and fumaronitrile were investigated with density functional theory (M06-2X/6-311G(d,p)). The activation free energies for the Diels-Alder reactions of cyclic 1-azadienes are 10-14 kcal mol -1 higher than those of cyclic 2-azadienes, and the reaction free energies are 17-20 kcal mol -1 more endergonic. The distortion/interaction model shows that the increased activation energies of cyclic 1-azadienes originate from increased transition state distortion energies and unfavorable interaction energies, arising from addition to the nitrogen terminus of the C═N bond.

Chemical composition of essential oil and antimicrobial properties of Chrysantemum coronarium (Asteraceae

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I. V. Ivashchenko

2017-03-01

Full Text Available Garland chrysanthemum (Chrysanthemum coronarium L., or edible chrysanthemum, is a valuable food, medicinal, decorative plant, containing a considerable amount of biologically active substances. The herb is widely used as a dietary food in South-East Asia, whereas in spite of being spread throughout Ukraine, it is known there rather as a decorative than a vegetable plant. Introductory studies of C. coronarium were conducted on experimental plots at the Botanical Gardens of Zhytomyr National Agroecological University, which is located in Ukrainian Polesia. Chromatographic analysis of the essential oil composition was performed on the gas-liquid chromatographer Agilent Technologies 6890 with mass spectrometric detector 5973. The material for chromatographic studies was represented by C. coronarium inflorescences. The antimicrobial properties of the ethanolic extract from the areal parts of C. coronarium were studied on test-cultures, collected from the Ukrainian Collection of Microorganisms (UCM, Institute of Microbiology and Virology of NAS Ukraine, the test-cultures being: Escherichia coli UCM B-906 (ATCC 25922, Staphilococcus aureus UCM B-904 (ATCC 25923, Pseudomonas aeruginosa UCM B-900 (ATCC 9027, Candida albicans UCM Y-1918 (ATCC 885-653. The antimicrobial effect of the investigated substances was studied by the method of serial successive dilutions which determined minimal inhibitory concentration (MIC and minimal bactericidal concentration (MBC. This article shows the results of chromatographic analysis of essential oil obtained from C. coronarium inflorescences and focuses on antimicrobial activity of the herb against the test cultures of the following microorganisms: E. coli, S. aureus, P. aeruginosa, C. albicans. In the essential oil 26 compounds have been determined, 23 of which have been identified, the major components being: chrysanthemyl acetate (24.4%, chrysanthemol (21.8%, chrysanthenyl acetate (7.6%, camphor (7.3%, �

Development of Direct Reversed-Phase High Performance liquid chromatographic method for quantitative determination of gabapentin in pharmaceutical dosage

International Nuclear Information System (INIS)

Hassan, W.; Zaman, B.; Rahman, S.; Rahman, A.U.; Ali, N.; Mohammadzai, I.U.

2012-01-01

The objective of the present work was to develop and validate a rapid analytical method for quantitative determination of Gabapentin in pharmaceutical dosage tablets and capsules. An accurate, simple, and sensitive reversed-phase high performance liquid chromatographic (HPLC) method, UV detection at 215 nm and flow rate at 1.0 ml/min has been developed. Isocratic elution was used instead of gradient elution to reduce the time and cost of serial analysis. The mobile phase was a mixture of water and methanol (HPLC grade). The retention time (Rt) of Gabapentin was 4.681 +- 0.013 minutes. Recovery, Precision, accuracy, and linearity were determined for the stated method. The calibration curve was linear and the correlation coefficient was 0.9996. There was no chromatographic interference from other excipients present in dosage form. The method was validated appropriately and successfully used for determination of Gabapentin in Pharmaceutical formulations. (author)

Performance characteristics of bioassay, radioenzymatic assay, homogeneous enzyme immunoassay, and high-performance liquid chromatographic determination of serum gentamicin

International Nuclear Information System (INIS)

Delaney, C.J.; Opheim, K.E.; Smith, A.L.; Plorde, J.J.

1982-01-01

We compared the accuracy, precision, and between-method error of the microbiological assay, the radioenzymatic assay, the homogeneous enzyme immunoassay, and the high-performance liquid chromatographic assay for the quantitation of gentamicin in serum. Precision and accuracy were evaluated by reference samples prepared to contain 0.0 to 32.7 micrograms of gentamicin per ml. Correlations between the methods utilized patient sera with gentamicin concentrations ranging from 0.6 to 13.3 micrograms/ml. All methods were reliable within acceptable limits for routine clinical use; intermethod correlation coefficients exceeded 0.96. Relative to the microbiological assay, the alternative methods offer the advantage of rapid analysis. The elapsed times for acquiring data on a set of 10 specimens under routine operating conditions were 0.5 h by the enzyme immunoassay, 4 h by the radioenzymatic assay, 5 h by the high-performance liquid chromatographic assay, and 10 h by the microbiological assay

Multidimensional High-Resolution Gas Chromatographic Investigations of Hydrocarbon Fuels and Various Turbine Engine Fuel Precursors.

Science.gov (United States)

1985-08-01

time were spurious transits observed during the recording of the chromatographic output data. *Packaged gas purification filters supplied by Alltech ... Alltech ) that were needed for these unusual installations. When the column diameters were small and of comparable size, the assembly attach- ments at...into an MDGC system has definite advantages as separations can be made faster and with greater detectability. However, specific precautions must be

A new modeling strategy for third-order fast high-performance liquid chromatographic data with fluorescence detection. Quantitation of fluoroquinolones in water samples.

Science.gov (United States)

Alcaráz, Mirta R; Bortolato, Santiago A; Goicoechea, Héctor C; Olivieri, Alejandro C

2015-03-01

Matrix augmentation is regularly employed in extended multivariate curve resolution-alternating least-squares (MCR-ALS), as applied to analytical calibration based on second- and third-order data. However, this highly useful concept has almost no correspondence in parallel factor analysis (PARAFAC) of third-order data. In the present work, we propose a strategy to process third-order chromatographic data with matrix fluorescence detection, based on an Augmented PARAFAC model. The latter involves decomposition of a three-way data array augmented along the elution time mode with data for the calibration samples and for each of the test samples. A set of excitation-emission fluorescence matrices, measured at different chromatographic elution times for drinking water samples, containing three fluoroquinolones and uncalibrated interferences, were evaluated using this approach. Augmented PARAFAC exploits the second-order advantage, even in the presence of significant changes in chromatographic profiles from run to run. The obtained relative errors of prediction were ca. 10 % for ofloxacin, ciprofloxacin, and danofloxacin, with a significant enhancement in analytical figures of merit in comparison with previous reports. The results are compared with those furnished by MCR-ALS.

A study of the barrier properties of polyethylene coated with a nanocellulose/magnetite composite film

Directory of Open Access Journals (Sweden)

Đorđević Nenad

2016-01-01

Full Text Available The morphological, thermal and barrier properties of low-density polyethylene/polycaprolactone-modified nanocellulose hybrid materials were investigated in this paper. Nanonocelulose/magnetite (NC-Fe3O4 nanocomposite and maleic acid functionalized NC/magnetite (NCMA-Fe3O4 nanocomposite were prepared and used as filler at various concentrations (5, 10 and 15 wt. % in polycaprolactone (PCL layer. PE was coated with PCL/NC/magnetite layer. The addition of the filler did not unfavorably affect the inherent properties of the polymer, especially its barrier properties. Oxygen permeation measurements show that the oxygen barrier properties of magnetite enriched PCL film were improved due to chemical activity of added material. The highest level of barrier capacity was observed for PE samples coated with PCL based composite with NCMA-Fe3O4 micro/-nanofiller, which implies the significant contribution of nanocellulose surface modification with maleic anhydride residue to improved barrier properties. [Projekat Ministarstva nauke Republike Srbije, br. III45019 i br. OI172013

Incorporation of metal-organic framework HKUST-1 into porous polymer monolithic capillary columns to enhance the chromatographic separation of small molecules.

Science.gov (United States)

Yang, Shengchao; Ye, Fanggui; Lv, Qinghui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

2014-09-19

Metal-organic framework (MOF) HKUST-1 nanoparticles have been incorporated into poly(glycidyl methacrylate-co-ethylene dimethacrylate) (HKUST-1-poly(GMA-co-EDMA)) monoliths to afford stationary phases with enhanced chromatographic performance of small molecules in the reversed phase capillary liquid chromatography. The effect of HKUST-1 nanoparticles in the polymerization mixture on the performance of the monolithic column was explored in detail. While the bare poly(GMA-co-EDMA) monolith exhibited poor resolution (RsHKUST-1 nanoparticles to the polymerization mixture provide high increased resolution (Rs≥1.3) and high efficiency ranged from 16,300 to 44,300plates/m. Chromatographic performance of HKUST-1-poly(GMA-co-EDMA) monolith was demonstrated by separation of various analytes including polycyclic aromatic hydrocarbons, ethylbenzene and styrene, phenols and aromatic acids using a binary polar mobile phase (CH3CN/H2O). The HKUST-1-poly(GMA-co-EDMA) monolith displayed enhanced hydrophobic and π-π interaction characteristics in the reversed phase separation of test analytes compared to the bare poly(GMA-co-EDMA) monolith. The experiment results showed that HKUST-1-poly(GMA-co-EDMA) monoliths are an alternative to enhance the chromatographic separation of small molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

Effects of γ-irradiation on caprolactam level from multilayer PA-6 films for food packaging: Development and validation of a gas chromatographic method

International Nuclear Information System (INIS)

Araujo, Henrique Peres; Felix, Juliana Silva; Manzoli, Jose Eduardo; Padula, Marisa; Monteiro, Magali

2008-01-01

A gas chromatographic method to determine caprolactam in multilayer PA-6 films used for meat foodstuffs and cheese was developed and validated. A wide linear range (0.8-400 μg/ml), RSD≤4.1% and recovery higher than 90.0% were obtained for the chromatographic system, while precision and accuracy of the method showed RSD≤3.8%, recovery from 95.5-100.0% and LOQ of 32 μg/g. Irradiated (3, 7 and 12 kGy) and non-irradiated commercial films were analyzed. Most of them increased caprolactam levels with the increase of irradiation doses

Effects of {gamma}-irradiation on caprolactam level from multilayer PA-6 films for food packaging: Development and validation of a gas chromatographic method

Energy Technology Data Exchange (ETDEWEB)

Araujo, Henrique Peres; Felix, Juliana Silva [Department of Food and Nutrition, School of Pharmaceutical Science, Sao Paulo State University, PO Box 502, 14801-902 Araraquara, SP (Brazil); Manzoli, Jose Eduardo [Nuclear and Energetic Research Institute (IPEN), Sao Paulo, SP (Brazil); Padula, Marisa [Packaging Technology Center/Food Technology Institute (CETEA/ITAL), Campinas, SP (Brazil); Monteiro, Magali [Department of Food and Nutrition, School of Pharmaceutical Science, Sao Paulo State University, PO Box 502, 14801-902 Araraquara, SP (Brazil)], E-mail: monteiro@fcfar.unesp.br

2008-07-15

A gas chromatographic method to determine caprolactam in multilayer PA-6 films used for meat foodstuffs and cheese was developed and validated. A wide linear range (0.8-400 {mu}g/ml), RSD{<=}4.1% and recovery higher than 90.0% were obtained for the chromatographic system, while precision and accuracy of the method showed RSD{<=}3.8%, recovery from 95.5-100.0% and LOQ of 32 {mu}g/g. Irradiated (3, 7 and 12 kGy) and non-irradiated commercial films were analyzed. Most of them increased caprolactam levels with the increase of irradiation doses.

Chromatographic separation and detection of contaminants from whole milk powder using a chitosan-modified silver nanoparticles surface-enhanced Raman scattering device.

Science.gov (United States)

Li, Dan; Lv, Di Y; Zhu, Qing X; Li, Hao; Chen, Hui; Wu, Mian M; Chai, Yi F; Lu, Feng

2017-06-01

Methods for the on-site analysis of food contaminants are in high demand. Although portable Raman spectroscopy is commonly used to test food on-site, it can be challenge to achieve this goal with rapid detection and inexpensive substrate. In this study, we detected trace food contaminants in samples of whole milk powder using the methods that combined chromatography with surface-enhanced Raman scattering detection (SERS). We developed a simple and efficient technique to fabricate the paper with chitosan-modified silver nanoparticles as a SERS-active substrate. The soaking time of paper and the concentration of chitosan solution were optimized for chromatographic separation and SERS detection. We then studied the separation properties for real applications including complex sample matrices, and detected melamine at 1mg/L, dicyandiamide at 100mg/L and sodium sulfocyanate at 10mg/L in whole milk powder. As such, our methods have great potential for field-based detection of milk contaminants. Copyright © 2016 Elsevier Ltd. All rights reserved.

The functional and biological properties of whey proteins: prospects for the development of functional foods

Directory of Open Access Journals (Sweden)

H. J. T. KORHONEN

2008-12-01

Full Text Available Advances in processing technologies and the accumulation of scientific data on the functional and biological properties of whey components have contributed to the growing commercial valuation of cheese whey over the last decade. New membrane separation and chromatographic techniques have made it possible to fractionate and enrich various components of whey more efficiently than before. The specific properties of these components can now be examined in greater detail and new applications developed accordingly. The utilisation of cheese whey is evolving into a new industry producing a multitude of purified ingredients for numerous purposes. The most significant areas of R&D related to whey proteins include functional foods, the rheological properties of foodstuffs, and biopharmaceuticals.

Different Spectrophotometric and Chromatographic Methods for Determination of Mepivacaine and Its Toxic Impurity.

Science.gov (United States)

Abdelwahab, Nada S; Fared, Nehal F; Elagawany, Mohamed; Abdelmomen, Esraa H

2017-09-01

Stability-indicating spectrophotometric, TLC-densitometric, and ultra-performance LC (UPLC) methods were developed for the determination of mepivacaine HCl (MEP) in the presence of its toxic impurity, 2,6-dimethylanaline (DMA). Different spectrophotometric methods were developed for the determination of MEP and DMA. In a dual-wavelength method combined with direct spectrophotometric measurement, the absorbance difference between 221.4 and 240 nm was used for MEP measurements, whereas the absorbance at 283 nm was used for measuring DMA in the binary mixture. In the second-derivative method, amplitudes at 272.2 and 232.6 nm were recorded and used for the determination of MEP and DMA, respectively. The developed TLC-densitometric method depended on chromatographic separation using silica gel 60 F254 TLC plates as a stationary phase and methanol-water-acetic acid (9 + 1 + 0.1, v/v/v) as a developing system, with UV scanning at 230 nm. The developed UPLC method depended on separation using a C18 column (250 × 4.6 mm id, 5 μm particle size) as a stationary phase and acetonitrile-water (40 + 60, v/v; pH 4 with phosphoric acid) as a mobile phase at a flow rate of 0.4 mL/min, with UV detection at 215 nm. The chromatographic run time was approximately 1 min. The proposed methods were validated with respect to International Conference on Harmonization guidelines regarding precision, accuracy, ruggedness, robustness, and specificity.

Spectroscopic and chromatographic characterisation of a pentafluorophenylpropyl silica phase end-capped in supercritical carbon dioxide as a reaction solvent.

Science.gov (United States)

Ashu-Arrah, Benjamin A; Glennon, Jeremy D; Albert, Klaus

2013-07-12

This research uses solid-state nuclear magnetic resonance (NMR) spectroscopy to characterise the nature and amount of different surface species, and chromatography to evaluate phase properties of a pentafluorophenylpropyl (PFPP) bonded silica phase prepared and end-capped using supercritical carbon dioxide (sc-CO2) as a reaction solvent. Under sc-CO2 reaction conditions (at temperature of 100 °C and pressure of 414 bar), a PFPP silica phase was prepared using 3-[(pentafluorophenyl)propyldimethylchlorosilane] within 1h. The bonded PFPP phase was subsequently end-capped with bis-N,O-trimethylsilylacetamide (BSA), hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) within 1h under the same sc-CO2 reaction conditions (100 °C/4141 bar). Elemental microanalysis, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) were used to provide support data to solid-state NMR and chromatographic evaluation. Results revealed a surface coverage of 2.2 μmol/m(2) for the non-end-capped PFPP silica phase while the PFPP phase end-capped with BSA gave a higher surface coverage (3.9 μmol/m(2)) compared to HMDS (2.9 μmol/m(2)) and TMCS (2.8 μmol/m(2)). (29)Si CP/MAS NMR analysis of the PFPP end-capped with BSA shows a significant decrease in the amount of Q(3) (free silanols) and Q(4) (siloxane groups) species, coupled with the absence of the most reactive Q(2) (geminal silanols) in addition to increased amount of a single resonance peak centred at +13 ppm (MH) corresponding to -Si-O-*Si-CH3 bond. (13)C CP/MAS NMR shows the resonance corresponding to the propyl linkage (CH3CH2CH2-) and methyl groups (Si(CH3)n) confirming successful silanisation and endcapping reactions in sc-CO2. Chromatographic evaluation of the BSA end-capped PFPP phase with Neue text mixture revealed improved chromatographic separation as evidenced in the enhanced retention of hydrophobic markers and decreased retention for basic solutes. Moreover, chromatography revealed a change in

A purge-and-trap capillary column gas chromatographic method for the measurement of halocarbons in water and air

Energy Technology Data Exchange (ETDEWEB)

Happell, J.D.; Wallace, D.W.R.; Wills, K.D.; Wilke, R.J.; Neill, C.C.

1996-06-01

This report describes an automated, accurate, precise and sensitive capillary column purge- and -trap method capable of quantifying CFC-12, CFC-11, CFC-113, CH{sub 3}CCL{sub 3}, and CCL{sub 4} during a single chromatographic analysis in either water or gas phase samples.

Liquid chromatographic method for simultaneous determination of citalopram with NSAIDs in bulk drug, pharmaceutical formulation and human serum

International Nuclear Information System (INIS)

Ali, S.N.; Akram, S.

2017-01-01

A high performance liquid chromatographic method was developed and validated to simultaneously quantify citalopram with piroxicam, celecoxib and diclofenac sodium. Chromatographic analysis was performed at ambient temperature using Shimadzu Shim-pack CLC-ODS (M) 25M column linked to a UV-visible detector adjusted at 230 nm, employing 80:20 (v/v) methanol: water (pH 3.5) as mobile phase with flow rate 1.0 mL min-1. Validation was performed in the ranges 0.6-20, 0.9-28, 0.6-20 and 1.0-32 mu g mL-1 with lowest level corresponding to detection limit 16.45, 23.33, 27.66 and 14.44 ng mL-1 respectively. With-in the day precision ranged from 0.14-1.67% and between-day precision from 0.40-1.50%, accuracies were 99.61-100.86%. The analytes were successfully detected without any observable interference in pharmaceutical formulation and human serum samples demonstrating effectiveness of method. (author)

An innovative, simple, fast, and less toxic high-performance liquid chromatographic method for determination of prednisone in capsules

Directory of Open Access Journals (Sweden)

Pedro Henrique Reis da Silva

2017-06-01

Full Text Available ABSTRACT Prednisone is an anti-inflammatory steroid drug widely used in clinical practice. However, no high-performance liquid chromatographic (HPLC method has been described in the literature for the determination of prednisone in capsules until now. Thus, an HPLC method was developed using a C18 (250x4.0, 5 µm column, with methanol:water (70:30 as mobile phase at a flow rate of 1 mL/min and detection at 240 nm. The developed method was validated following current Brazilian legislation. Additionally, linearity was assessed by evaluating the assumptions of normality, homoscedasticity, and independency of residuals, and the fit to the linear model. The method showed linearity (r2>0.99 over the range of 14.0-26.0 µg/mL, selectivity, precision (RSD<2.0%, robustness, and accuracy (average recovery of 100.05%. The chromatographic procedure was applied for assay and uniformity content determination of three different batches of prednisone capsules, showing to be suitable for their quality control.

The Association of Unfavorable Traffic Events and Cannabis Usage: A Meta-Analysis

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Sorin Hostiuc

2018-02-01

Full Text Available Background: In the last years were published many epidemiological articles aiming to link driving under the influence of cannabis (DUIC with the risk of various unfavorable traffic events (UTEs, with sometimes contradictory results.Aim: The primary objective of this study was to analyze whether there is a significant association between DUIC and UTEs.Materials and Methods: We used two meta-analytical methods to assess the statistical significance of the effect size: random-effects model and inverse variance heterogeneity model.Results: Twenty-four studies were included in the meta-analysis. We obtained significant increases in the effect size for DUIC tested through blood analysis, with an odds ratio (OR of 2.27 and a confidence interval (CI between 1.36 and 3.80; death as an outcome, with an OR of 1.56 and a CI between 1.16 and 2.09; and case–control as the type of study, with an OR of 1.99 and a CI between 1.05 and 3.80. Publication bias was very high.Conclusion: Our analysis suggests that the overall effect size for DUIC on UTEs is not statistically significant, but there are significant differences obtained through subgroup analysis. This result might be caused by either methodological flaws (which are often encountered in articles on this topic, the indiscriminate employment of the term “cannabis use,” or an actual absence of an adverse effect. When a driver is found, in traffic, with a positive reaction suggesting cannabis use, the result should be corroborated by either objective data regarding marijuana usage (like blood analyses, with clear cut-off values, or a clinical assessment of the impairment, before establishing his/her fitness to drive.

The Association of Unfavorable Traffic Events and Cannabis Usage: A Meta-Analysis

Directory of Open Access Journals (Sweden)

Sorin Hostiuc

2018-02-01

Full Text Available Background: In the last years were published many epidemiological articles aiming to link driving under the influence of cannabis (DUIC with the risk of various unfavorable traffic events (UTEs, with sometimes contradictory results.Aim: The primary objective of this study was to analyze whether there is a significant association between DUIC and UTEs.Materials and Methods: We used two meta-analytical methods to assess the statistical significance of the effect size: random-effects model and inverse variance heterogeneity model.Results: Twenty-four studies were included in the meta-analysis. We obtained significant increases in the effect size for DUIC tested through blood analysis, with an odds ratio (OR of 1.97 and a confidence interval (CI between 1.35 and 2.87; death as an outcome, with an OR of 1.56 and a CI between 1.16 and 2.09; and case–control as the type of study, with an OR of 1.99 and a CI between 1.05 and 3.80. Publication bias was very high.Conclusion: Our analysis suggests that the overall effect size for DUIC on UTEs is not statistically significant, but there are significant differences obtained through subgroup analysis. This result might be caused by either methodological flaws (which are often encountered in articles on this topic, the indiscriminate employment of the term “cannabis use,” or an actual absence of an adverse effect. When a driver is found, in traffic, with a positive reaction suggesting cannabis use, the result should be corroborated by either objective data regarding marijuana usage (like blood analyses, with clear cut-off values, or a clinical assessment of the impairment, before establishing his/her fitness to drive.

Hydration properties of natural and synthetic DNA sequences with methylated adenine or cytosine bases in the R.DpnI target and BDNF promoter studied by molecular dynamics simulations

Science.gov (United States)

Shanak, Siba; Helms, Volkhard

2014-12-01

Adenine and cytosine methylation are two important epigenetic modifications of DNA sequences at the levels of the genome and transcriptome. To characterize the differential roles of methylating adenine or cytosine with respect to their hydration properties, we performed conventional MD simulations and free energy perturbation calculations for two particular DNA sequences, namely the brain-derived neurotrophic factor (BDNF) promoter and the R.DpnI-bound DNA that are known to undergo methylation of C5-methyl cytosine and N6-methyl adenine, respectively. We found that a single methylated cytosine has a clearly favorable hydration free energy over cytosine since the attached methyl group has a slightly polar character. In contrast, capping the strongly polar N6 of adenine with a methyl group gives a slightly unfavorable contribution to its free energy of solvation. Performing the same demethylation in the context of a DNA double-strand gave quite similar results for the more solvent-accessible cytosine but much more unfavorable results for the rather buried adenine. Interestingly, the same demethylation reactions are far more unfavorable when performed in the context of the opposite (BDNF or R.DpnI target) sequence. This suggests a natural preference for methylation in a specific sequence context. In addition, free energy calculations for demethylating adenine or cytosine in the context of B-DNA vs. Z-DNA suggest that the conformational B-Z transition of DNA transition is rather a property of cytosine methylated sequences but is not preferable for the adenine-methylated sequences investigated here.

Brazilian organic sugarcane spirits: Physicochemical and chromatographic profile

Directory of Open Access Journals (Sweden)

Felipe Cimino Duarte

Full Text Available ABSTRACT There has been a growing demand for products from organic agriculture for the food market. Brazil leads the production of sugarcane spirits and produces about 1.6 billion liters/year. New technologies have been sought throughout the supply chain to improve production, and organic raw material has been used in the production of sugar cane for the production of beverages. This study aimed to define the physicochemical and chromatographic profiles of eleven organic sugarcane spirits samples from various Brazilian states. The secondary components and contaminants were identified and quantified through physicochemical analyses, HPLC and gas chromatography (GC. A significant percentage of the organic sugarcane spirits samples contained concentrations of components that were above the limits required by the Ministry of Agriculture, Livestock and Provisioning (MAPA, specifically the esters (18.20%, copper and dry extract (9.10%. This contamination is caused by bad conditions employed during the production process, which are not in compliance with the good manufacturing practices determined and legislated by Brazilian law.

Comprehensive two-dimensional liquid chromatographic analysis of poloxamers.

Science.gov (United States)

Malik, Muhammad Imran; Lee, Sanghoon; Chang, Taihyun

2016-04-15

Poloxamers are low molar mass triblock copolymers of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO), having number of applications as non-ionic surfactants. Comprehensive one and two-dimensional liquid chromatographic (LC) analysis of these materials is proposed in this study. The separation of oligomers of both types (PEO and PPO) is demonstrated for several commercial poloxamers. This is accomplished at the critical conditions for one of the block while interaction for the other block. Reversed phase LC at CAP of PEO allowed for oligomeric separation of triblock copolymers with regard to PPO block whereas normal phase LC at CAP of PPO renders oligomeric separation with respect to PEO block. The oligomeric separation with regard to PEO and PPO are coupled online (comprehensive 2D-LC) to reveal two-dimensional contour plots by unconventional 2D IC×IC (interaction chromatography) coupling. The study provides chemical composition mapping of both PEO and PPO, equivalent to combined molar mass and chemical composition mapping for several commercial poloxamers. Copyright © 2016 Elsevier B.V. All rights reserved.

Chromatographic separation of low-temperature tar. Part III

Energy Technology Data Exchange (ETDEWEB)

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

1955-01-01

Experiments with crude phenolic mixtures in benzene-MeOH over an alumina chromatographic column are reported. The most effective separation into crude fractions was obtained from a petroleum-ether solution with benzene and benzene-MeOH elution. These fractions are analyzed by paper chromatography. R/sub f/ values for 29 phenols and benzoic acid from water-saturated AmOH are given. Folin-Denis reagent and ultraviolet absorption is used for identification of the phenolic compounds. R/sub f/ values for monohydroxy compounds are larger than 0.9, dihydroxy 0.80 to 0.9, trihydroxy 0.6, hydroxytoluic acids 0.39 to 0.56. R/sub f/ values of Na and K salts are different from those of the free phenols. Tests in aqueous solution near 0/sup 0/ gave important results. R/sub f/ values of the less polar materials decrease and less material is lost through evaporation, smaller and sharper spots are obtained and liquids move at a more even rate. A series of isomeric alkyl phenols is reported; ortho alkyl groups decrease the migration rate most effectively.

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.

A mobile automatic gas chromatograph system to measure CO2, CH4 and N2O fluxes from soil in the field

International Nuclear Information System (INIS)

Silvola, J.; Martikainen, P.; Nykaenen, H.

1992-01-01

A caravan has been converted into mobile laboratory for measuring fluxes of CO 2 , CH 4 and N 2 O from the soil in the field. The caravan was equipped with a gas chromatograph fitted with TC-, FI- and EC-detectors, and a PC controlled data logger. The gas collecting chambers can be used up to 50 m from the caravan. The closing and opening of the chambers, as well as the flows of sample gases from chambers to the gas chromatograph. is pneumatically regulated. Simultaneous recordings of temperature, light intensity and the depth of water table are made. The system has been used for two months in 1992, and some preliminary results are presented

Preparation of chromatographic and solid-solvent extraction 99mTc generators using gel-type targets

International Nuclear Information System (INIS)

Le Van So

2000-01-01

We have studied two types of targets zirconium-molybdate (ZrMo) and titanium-molybdate (TiMo) prepared by precipitating reaction between ammonium-molybdate and zirconium-chloride or titanium-chloride solutions, respectively. Other types of targets were also prepared by co-precipitating ZrMo or TiMo with hydrous manganese-dioxide, hydrous silica, and hydrous titanium-dioxide or by impregnated ZrMo or TiMo with Iodate anions. The results on extraction of Tc-99m from neutron irradiated TiMo solid phase using solvents such as MEK, aceton, ethylic ether, chloroform, etc showed that separation yield (SY) of Tc-99m in case of aceton extraction was from 70% to 80% and in other cases non higher than 40%. The Tc-99m elution curves and column kinetic in case of aceton extraction (after evaporation of aceton and recovery of Tc-99m in 0,9% NaCl solution) was superior than in case chromatographic generator using saline eluant. As result obtained, two types of generators were successfully prepared and put into use: Chromatographic generator using titanium-molybdate target as packing material and saline as eluant. Solid-solvent extraction 99m Tc generator using titanium-molybdate target (as solid phase) and aceton as extracting solvent. (author)

Choline chloride-based deep eutectic solvents as additives for optimizing chromatographic behavior of caffeic acid

International Nuclear Information System (INIS)

Li, Guizhen; Zhu, Tao; Lei, Yingjie

2015-01-01

A series of deep eutectic solvents (DESs) were prepared using glycerol and choline chloride (ChCl), and Fourier transform infrared spectrometer (FT-IR) was used to analyze the spectra of glycerol, choline chloride and DESs based on glycerol and choline chloride. Then DESs were used as the additives of mobile phase to optimize chromatographic behavior of caffeic acid in high performance liquid chromatography (HPLC). A 17-run Box-Behnken design (BBD) was employed to evaluate effect of DESs as additives by analyzing the maximum theoretical plate number. Three factors, reaction temperature (60 .deg. C, 80 .deg. C, 100 .deg. C), molar ratio of glycerol and choline chloride (2 : 1, 3 : 1, 4 : 1, n/n), and volume percent of additives (0.05%, 0.10%, 0.15%, v/v), were investigated in BBD. The optimum experiment condition was that of reaction temperature (80 .deg. C), molar ratio of glycerol and ChCl (3 : 1, n/n), and volume percent of additive (0.10%, v/v). The mean chromatographic theoretical plate number of the caffeic acid this condition was 1567.5, and DESs as additives shorten the retention time and modify the chromatogram shape, proving DESs as additives for effective theoretical plate number and column efficiency in HPLC.

Choline chloride-based deep eutectic solvents as additives for optimizing chromatographic behavior of caffeic acid

Energy Technology Data Exchange (ETDEWEB)

Li, Guizhen; Zhu, Tao; Lei, Yingjie [Tianjin University of Technology, Tianjin (China)

2015-10-15

A series of deep eutectic solvents (DESs) were prepared using glycerol and choline chloride (ChCl), and Fourier transform infrared spectrometer (FT-IR) was used to analyze the spectra of glycerol, choline chloride and DESs based on glycerol and choline chloride. Then DESs were used as the additives of mobile phase to optimize chromatographic behavior of caffeic acid in high performance liquid chromatography (HPLC). A 17-run Box-Behnken design (BBD) was employed to evaluate effect of DESs as additives by analyzing the maximum theoretical plate number. Three factors, reaction temperature (60 .deg. C, 80 .deg. C, 100 .deg. C), molar ratio of glycerol and choline chloride (2 : 1, 3 : 1, 4 : 1, n/n), and volume percent of additives (0.05%, 0.10%, 0.15%, v/v), were investigated in BBD. The optimum experiment condition was that of reaction temperature (80 .deg. C), molar ratio of glycerol and ChCl (3 : 1, n/n), and volume percent of additive (0.10%, v/v). The mean chromatographic theoretical plate number of the caffeic acid this condition was 1567.5, and DESs as additives shorten the retention time and modify the chromatogram shape, proving DESs as additives for effective theoretical plate number and column efficiency in HPLC.

Facile room-temperature solution-phase synthesis of a spherical covalent organic framework for high-resolution chromatographic separation.

Science.gov (United States)

Yang, Cheng-Xiong; Liu, Chang; Cao, Yi-Meng; Yan, Xiu-Ping

2015-08-07

A simple and facile room-temperature solution-phase synthesis was developed to fabricate a spherical covalent organic framework with large surface area, good solvent stability and high thermostability for high-resolution chromatographic separation of diverse important industrial analytes including alkanes, cyclohexane and benzene, α-pinene and β-pinene, and alcohols with high column efficiency and good precision.

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.

Chromatographic separation of metal ions by means of paper treated with trioctyl - phosphate, Annex 7

Energy Technology Data Exchange (ETDEWEB)

Cvjeticanin, N M; Cvoric, J D; Obrenovic-Paligoric, I D [Institute of Nuclear Sciences Boris Kidric, Laboratorija za visoku aktivnost, Vinca, Beograd (Serbia and Montenegro)

1963-12-15

This chromatographic behaviour of uranium, thorium and some other metal ions and long-lived fission products was investigated on paper treated with trioctyl-phosphate. Hydrochloric, nitric, sulphuric and perchloric acids in concentrations of 0.1-10 N were used as the elution agents. The R{sub f} values of the ions investigated, which show the possibility of the inter separation of some cations, are given as a function of the concentration of acids (author)

Characterization of a chromatographic column for the production of 90Sr

International Nuclear Information System (INIS)

Fornaciari Iljadica, Maria C.; Furnari, Juan C.; Cohen, Isaac M.

2003-01-01

The experiments carried out with the objective of developing a method for 90 Sr production, associated to that of 99 Mo from 235 U fission, which is routinely performed at Centro Atomico Ezeiza, Comision Nacional de Energia Atomica, are described. The project consists of strontium separation from a nitric solution containing uranium and a variety of fission products, by retention and subsequent elution in selective chromatographic columns. Both these columns and the conditions for their use in a routine production process have been characterized. The experiments show good Sr-Ba separation, high concentration of activity for the obtained 90 Sr, and minimal losses; in addition, the non-existence of significant radiation damage, as a limiting factor of the separative capacity of the columns, has been verified. (author)

Chromatographic fingerprinting as a strategy to identify regulated plants in illegal herbal supplements.

Science.gov (United States)

Custers, D; Van Praag, N; Courselle, P; Apers, S; Deconinck, E

2017-03-01

Erectile dysfunction (ED) is a sexual disorder characterized by the inability to achieve or maintain a sufficiently rigid erection. Despite the availability of non-invasive oral treatment options, many patients turn to herbal alternatives. Furthermore, herbal supplements are increasingly gaining popularity in industrialized countries and, as a consequence, quality control is a highly important issue. Unfortunately, this is not a simple task since plants are often crushed and mixed with other plants, which complicates their identification by usage of classical approaches such as microscopy. The aim of this study was to explore the potential use of chromatographic fingerprinting to identify plants present in herbal preparations intended for the treatment of ED. To achieve this goal, a HPLC-PDA and a HPLC-MS method were developed, using a full factorial experimental design in order to acquire characteristic fingerprints of three plants which are potentially beneficial for treating ED: Epimedium spp., Pausinystalia yohimbe and Tribulus terrestris. The full factorial design demonstrated that for all three plant references a C8 column (250mm×4.6mm; 5µm particle size) is best suited; methanol and an ammonium formate buffer (pH 3) were found to be the best constituents for the mobile phase. The suitability of this strategy was demonstrated by analysing several self-made triturations in three different botanical matrices, which mimic the influential effects that could be expected when analysing herbal supplements. To conclude, this study demonstrates that chromatographic fingerprinting could provide a useful means to identify plants in a complex herbal mixture. Copyright © 2016 Elsevier B.V. All rights reserved.

Measurement uncertainty of liquid chromatographic analyses visualized by Ishikawa diagrams.

Science.gov (United States)

Meyer, Veronika R

2003-09-01

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 uncertainty calculation. In this case, it is at least necessary to consider the uncertainty of the purity of the reference material in addition to the precision data. The Ishikawa diagram is then very simple, and so is the uncertainty calculation. This advantage is given by the loss of information about the parameters that influence the measurement uncertainty.

Reconstruction of Nanoindustry Institutes in the Russian Federation in the Unfavorable Global Environment

Directory of Open Access Journals (Sweden)

Oleg Vasilyevich Inshakov

2015-12-01

Full Text Available Nanoindustry evolution is caused by the global extension of new technological mode, which requires the construction of effective institutes and mechanisms of regulating its subjects’ relations. In the conditions of unfavorable external environment and unsolved internal problems of Russian nanoindustry development, not only the role of basic nanoindustrialization institutes increases, but the problem of reconstructing their activity and prospective updating of institutions arises. Regardless of level and scale, forms and content, the institutional reconstruction will become a part of a rapid response to external changes and a component of strategic programming of Russian nanoindustry. The Russian government acted as a main institute of national nanoindustry development and support. New special-purpose/universal, financial/nonfinancial, formal/informal institutes, which make up the structure of target investment and resource supply of nanoindustry at various stages of its formation, become active agents of state policy in this sphere. This institutional system should reflect the level and type structure of nanoindustry, corresponding to its strategic perspective. An important role in overcoming negative trends in nanoindustry now belongs not to formal and corporate development institutes but to associative, initiative and complementary ones partially replacing the state as its substitutes. The authors describe the options of international financial funds and integration-type institutes’ reconstruction for Russian nanoindustry in current situation. The feasibility of orienting the construction of nanoindustry institutes to basic relationships of its subjects that ensures their relevance and effectiveness, is argued. The authors’ version of nanoindustry institutes classification is suggested for applying as a testing analyzer of institutes functioning in order to determine their reconstruction directions, identify and supplement missing links

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.

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

The development of a high performance liquid chromatograph with a sensitive on-stream radioactivity monitor for the analysis of 3H- and 14C-labelled gibberellins

International Nuclear Information System (INIS)

Reeve, D.R.; Yokota, T.; Nash, L.; Crozier, A.

1976-01-01

The development of a high performance liquid chromatograph for the separation of gibberellins is described. The system combines high efficiency, peak capacity, and sample capacity with rapid speed of analysis. In addition, the construction details of a sensitive on-stream radioactivity monitor are outlined. The overall versatility of the chromatograph has been demonstrated by the separation of a range of 3 H- and 14 C-labelled gibberellins and gibberellin precursors. The system also has considerable potential for the analysis of abscisic acid and acidic and neutral indoles. (author)

Combined Scintigraphy and Tumor Marker Analysis Predicts Unfavorable Histopathology of Neuroblastic Tumors with High Accuracy.

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Wolfgang Peter Fendler

Full Text Available Our aim was to improve the prediction of unfavorable histopathology (UH in neuroblastic tumors through combined imaging and biochemical parameters.123I-MIBG SPECT and MRI was performed before surgical resection or biopsy in 47 consecutive pediatric patients with neuroblastic tumor. Semi-quantitative tumor-to-liver count-rate ratio (TLCRR, MRI tumor size and margins, urine catecholamine and NSE blood levels of neuron specific enolase (NSE were recorded. Accuracy of single and combined variables for prediction of UH was tested by ROC analysis with Bonferroni correction.34 of 47 patients had UH based on the International Neuroblastoma Pathology Classification (INPC. TLCRR and serum NSE both predicted UH with moderate accuracy. Optimal cut-off for TLCRR was 2.0, resulting in 68% sensitivity and 100% specificity (AUC-ROC 0.86, p < 0.001. Optimal cut-off for NSE was 25.8 ng/ml, resulting in 74% sensitivity and 85% specificity (AUC-ROC 0.81, p = 0.001. Combination of TLCRR/NSE criteria reduced false negative findings from 11/9 to only five, with improved sensitivity and specificity of 85% (AUC-ROC 0.85, p < 0.001.Strong 123I-MIBG uptake and high serum level of NSE were each predictive of UH. Combined analysis of both parameters improved the prediction of UH in patients with neuroblastic tumor. MRI parameters and urine catecholamine levels did not predict UH.

Reverse-Phase High-Performance Liquid Chromatographic Separation of Methylated and Non-Methylated Nucleic Acid Bases

OpenAIRE

Madyastha, Prema; Rao, Pratima; Deobagkar, DN; Madyastha, KM

1983-01-01

A high-performance liquid chromatographic sepration method is described for the detection of 5-methylcytosine and 6-methyladenine in nucleic acid ext. The bases were sepd. on a Waters $C18 \\mu$ Bondapak column with a water: methanol acetic acid system. Effluents were monitored by UV absorption at 254 nm. The bases were estd. by peak heights which are proportional to the amts. of the individual bases. The method is rapid, sensitive, easy to perform and reproducible.

Chromatographic determination of Fe chelated by ethylenediamine-N-(o-hydroxyphenylacetic)-N'-(p-hydroxyphenylacetic) acid in commercial EDDHA/Fe3+ fertilizers.

Science.gov (United States)

García-Marco, Sonia; Torreblanca, Ana; Lucena, Juan J

2006-02-22

EDDHA/Fe3+ chelates are the most common fertilizers used to solve Fe chlorosis in established crops. Commercial products contain two regioisomers, ethylenediamine-N,N'-bis(o-hydroxyphenylacetic) acid (o,o-EDDHA)/Fe3+ and ethylenediamine-N-(o-hydroxyphenylacetic)-N'-(p-hydroxyphenylacetic) acid (o,p-EDDHA)/Fe3+. Although several chromatographic methods exist for the determination of Fe3+ chelated by the o,o-EDDHA isomer, no method has been described for the quantification of Fe3+ chelated by o,p-EDDHA. In this work, factors that affect the behavior of o,p-EDDHA/Fe3+ in ion pair chromatography are reviewed: pH, ion pair reagent, and organic modifier. The best chromatographic performance was obtained with an aqueous mobile phase at pH 6.0 containing 35% acetonitrile and 5 mM tetrabutylammonium hydroxide under isocratic elution conditions. This method was applied to the quantification of commercial samples.

Ion-chromatographic determination of borates and sulfides with the use of a developing column

International Nuclear Information System (INIS)

Kolotilina, N.K.; Dolgonosov, A.M.

2005-01-01

Aspects of the sensitive and selective determination of borates and sulfides were considered. A method was proposed for substantially increasing the sensitivity of the ion-chromatographic determination of weak acids by their conversion into corresponding salts on an auxiliary column with a cation exchanger in the K form. It is demonstrated that the detection limit of the anions under consideration can be decreased to 5-10 μg/l and the selectivity of the method is sufficient for the determination of trace borates in strongly mineralized waters like sea water [ru

Chromatographic peak resolution using Microsoft Excel Solver. The merit of time shifting input arrays.

Science.gov (United States)

Dasgupta, Purnendu K

2008-12-05

Resolution of overlapped chromatographic peaks is generally accomplished by modeling the peaks as Gaussian or modified Gaussian functions. It is possible, even preferable, to use actual single analyte input responses for this purpose and a nonlinear least squares minimization routine such as that provided by Microsoft Excel Solver can then provide the resolution. In practice, the quality of the results obtained varies greatly due to small shifts in retention time. I show here that such deconvolution can be considerably improved if one or more of the response arrays are iteratively shifted in time.

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.

High-performance liquid chromatographic analysis of anthraquinone compounds in the Laurera benguelensis

Science.gov (United States)

Manojlović, N.; Marković, Z.; Gritsanapan, W.; Boonpragob, K.

2009-09-01

A high-performance liquid chromatographic (HPLC) method has been developed for the characterization of anthraquinone metabolites in extracts of the lichen Laurera benguelensis. With this method four anthraquinone derivatives 1,8-dihydroxy-3-methoxy-6-methylanthraquinone, 1,8-dihydroxy-3-formyl-6-methoxyanthraquinone, 1,8-dihydroxy-3-hydroxymethyl-6-methoxy-anthraquinone and 1,3,8-trihyroxy-6-methylanthraquinone can be analyzed. Components of lichen were detected by characteristic ultraviolet spectra and relative retention times. This is first report of phytochemical analysis of L. benguelensis. Importance of this research is in recognizing some new source (lichen and its extracts) as a natural emplacement of antioxidants because oxidation with free radicals or autooxidation is big problem for preservation of food products.

Frequent conjugative transfer accelerates adaptation of a broad-host-range plasmid to an unfavorable Pseudomonas putida host.

Science.gov (United States)

Heuer, Holger; Fox, Randal E; Top, Eva M

2007-03-01

IncP-1 plasmids are known to be promiscuous, but it is not understood if they are equally well adapted to various species within their host range. Moreover, little is known about their fate in bacterial communities. We determined if the IncP-1beta plasmid pB10 was unstable in some Proteobacteria, and whether plasmid stability was enhanced after long-term carriage in a single host and when regularly switched between isogenic hosts. Plasmid pB10 was found to be very unstable in Pseudomonas putida H2, and conferred a high cost (c. 20% decrease in fitness relative to the plasmid-free host). H2(pB10) was then evolved under conditions that selected for plasmid maintenance, with or without regular plasmid transfer (host-switching). When tested in the ancestral host, the evolved plasmids were more stable and their cost was significantly reduced (9% and 16% for plasmids from host-switched and nonswitched lineages, respectively). Our findings suggest that IncP-1 plasmids can rapidly adapt to an unfavorable host by improving their overall stability, and that regular conjugative transfer accelerates this process.

Chromatographic purification of neutron capture molybdenum-99 from cross-contaminant radionuclides

International Nuclear Information System (INIS)

Mostafa, M.A.M.

2011-01-01

Technetium-99m is called the work horse, for many reasons, in nuclear medicine diagnostic purposes. It is produced as the β - decay of 99 Mo radionuclide. Molybdenum-99 gel type generators are considered as a suitable alternative of the conventional chromatographic alumina columns loaded with fission molybdenum-99. 99 Mo neutron-capture is cross-contaminated with radionuclides originated from activation of chemical impurities in the Mo target such 60 C0, 65 Zn, 95 Zr, 175 Hf, 181 Hf, 86 Rb, 134 Cs, 141 Ce, 152 Eu, 140 La, 51 Cr, 124 Sb, 46 Sc, 54 Mn, 59 Fe and / or fast neutrons interactions with the stable isotopes of molybdenum such as 92m Nb, 95 Nb and 95 Zr. To prevent contamination of the eluted 99m Tc, successive purification methods were made. After complete dissolution of the irradiated target wrapped with thin Al foil in 5 M NaOH solution, hydrogen peroxide was added to start precipitation of Fe(OH) 3 . The formed Fe (III) minerals allow complete elimination of some radio contaminants from the molybdate solute such as 152 Eu, 140 La, 141 Ce, 45 Mn and 92m Nb in addition to partial elimination of 46 Sc, 60 Co and 59 Fe radionuclides. The remaining supernatant was acidified by concentrated nitric acid to ph 9.5 for precipitation of Al(OH) 3 with complete elimination of radio contaminants such as 95 Zr 175 Hf, 181 Hf, 65 Zn, 124 Sb, 51 Cr, 46 Sc, 60 Co and 59 Fe. 134 Cs and 86 Rb radionuclides were not affected by precipitation of Fe(OH) 3 or Al(OH) 3 . Chromatographic column of potassium nickel hexacyanoferrate (II) (KNHCF) has high affinity towards elimination of 134 Cs and 86 Rb radionuclides. Highly pure molybdate- 99 Mo solution was processed for preparation of zirconium molybdate gel generator with 99m Tc eluate of high radionuclidic, radiochemical and chemical purity suitable for use in medical purposes.

Liquid chromatographic determination of polyphenenols in czech beers during brewing proces

Directory of Open Access Journals (Sweden)

Chunsriimyatav Ganbaatar

2015-05-01

Full Text Available High performance liquid chromatographic (HPLC/UV method was adapted for simultaneous determination of seven polyphenols, including derivatives of benzoic (gallic and vanillic acids and cinnamic acids (p-coumaric, ferulic and sinapic acids, flavan-3-ols (catechin and flavonols (rutin in worts and beers at the various stages of the brewing process. Based on the semi-quantitative HPLC analysis, total polyphenols chromatographic index (TPCI was in the ranges of 5.18 - 19.4 mg/L and 7.37 - 20.7 mg/L for all worts and beers, respectively. The HPLC analyses showed that relatively high levels of (+-catechin and gallic acid were in all the worts and the beers, while the values were much lower for ferulic acid, rutin, vanillic acid, sinapic acid and p-coumaric acid. Polyphenols with relatively high concentrations, that were detected in all tested worts and beers, were gallic acid (1.29 - 4.75 mg/L resp. 2.59 - 4.97 mg/L, (+-catechin (1.66 - 7.95 mg/L resp. 4.70 - 10.0 mg/L and ferulic acid (0.41 - 4.53 mg/L resp. 1.05 - 2.87 mg/L. On the other side, the sinapic acid (0.72 - 1.59 mg/L resp. 0.72 - 2.5 mg/L, rutin (1.17 - 2.03 mg/L resp. 1.16 - 2.85 mg/L, p-coumaric acid (ND - 4.73 mg/L resp. ND - 1.44 mg/L and vanillic acid (ND - 1.52 mg/L resp. 0.75 - 1.81 mg/L were detected in lowest concentrations. In both, worts and beers investigated in this study, the changes in the contents of individual polyphenols were not uniform. In the case of some polyphenols, a decrease in the content was observed after boiling the worts with hops or after the main fermentation until maturation and filtration, but with some polyphenols, the concentrations were constant until the end of the process or even increased.

Column chromatographic separation of Y3+ from Sr2+ by polymeric ionizable crown ether resins

International Nuclear Information System (INIS)

Wood, D.J.; Elshani, S.; Wai, C.M.; Bartsch, R.A.; Huntley, M.; Hartenstein, S.

1993-01-01

Condensation polymers containing subunits of crown ether carboxylic acid monomers are effective stationary phases for the chromatographic separation of Y 3+ and Sr 2+ . The pH range and metal loading capacities for the resins have been determined under equilibrium conditions. The resin can be regenerated for repeated use without losing its separation capability. Altering the molecular structure of the monomer (sym-dibenzo-16-crown-5-oxyacetic acid) by an alkyl substitution on the macrocyclic cavity decreases the loading capacity of the resin

Large scale gas chromatographic demonstration system for hydrogen isotope separation

International Nuclear Information System (INIS)

Cheh, C.H.

1988-01-01

A large scale demonstration system was designed for a throughput of 3 mol/day equimolar mixture of H,D, and T. The demonstration system was assembled and an experimental program carried out. This project was funded by Kernforschungszentrum Karlsruhe, Canadian Fusion Fuel Technology Projects and Ontario Hydro Research Division. Several major design innovations were successfully implemented in the demonstration system and are discussed in detail. Many experiments were carried out in the demonstration system to study the performance of the system to separate hydrogen isotopes at high throughput. Various temperature programming schemes were tested, heart-cutting operation was evaluated, and very large (up to 138 NL/injection) samples were separated in the system. The results of the experiments showed that the specially designed column performed well as a chromatographic column and good separation could be achieved even when a 138 NL sample was injected

[Reversed-phase high-performance liquid chromatograph--application to serum aluminium monitoring].

Science.gov (United States)

Hoshino, H; Kaneko, E

1996-01-01

High-Performance Liquid Chromatography (HPLC) with the reversed-phase partition mode separation (including ion-pair one) towards metal chelate compounds prepared in an off-line fashion (precolumn chelation) is most versatile in terms of high sensitivity with base-line flatness, unique selectivity and cost effectiveness. The extraordinary toughness to the complicated matrices encountered in clinical testing is exemplified by the successful application to the aluminium monitoring of human serum samples. The A1 chelate with 2,2'-dihydroxyazobenzene is efficiently chromatographed on a LiChroCART RP-18 column using an aqueous methanol eluent (63.6 wt%) containing tetrabutylammonium bromide as an ion-pair agent. The serum concentration level of A1 down to 6 micrograms dm-3 is readily monitored without influences from iron, chyle and haemolysis.

Detection system for a gas chromatograph. [. cap alpha. -methylnaphthalene,. beta. -methylnapthalene

Science.gov (United States)

Hayes, J.M.; Small, G.J.

1982-04-26

A method and apparatus are described for the quantitative analysis of vaporizable compounds, and in particular of polycyclic aromatic hydrocarbons which may be induced to fluoresce. The sample to be analyzed is injected into a gas chromatography column and is eluted through a narrow orifice into a vacuum chamber. The free expansion of the eluted sample into the vacuum chamber creates a supersonic molecular beam in which the sample molecules are cooled to the extent that the excited vibrational and rotational levels are substantially depopulated. The cooled molecules, when induced to fluoresce by laser excitation, give greatly simplified spectra suitable for analytical purposes. The laser induced fluorimetry provides great selectivity, and the gas chromatograph provides quantitative transfer of the sample to the molecular beam. 3 figures, 2 tables.

Chromatographic studies of thorium(IV) and its extraction from monazite sand

International Nuclear Information System (INIS)

Bandyopadhyay, Arup; Roy, Uday Sankar

1998-01-01

A simple, rapid and selective method has been developed for reversed phase extraction chromatographic studies of Th IV with high molecular mass monocarboxylic acid (C 15 -C 16 ), SRS-100 as a stationary phase on a column of silica gel. Quantitative extraction of Th IV has been achieved in the pH range 4.8-5.5. The extracted Th IV has been stripped with 1:1 (v/v) mixture of 0.2 M HNO 3 and 0.2 M NaNO 3 and estimated spectrophotometrically. The effect of variables as pH, stripping agents, flow rate on extraction and elution have been studied. Th IV has been separated from various commonly associated elements in binary and synthetic multicomponent mixtures. The method has been applied successfully for the extraction of thorium from monazite sand. (author)

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis

OpenAIRE

Kshirsagar, Parthraj R.; Hegde, Harsha; Pai, Sandeep R.

2016-01-01

Background and Aim: This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. Materials and Methods: 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. Results: Contaminant peak was detected in methanol stored in polypropylene m...

Physical Properties of Niobium and Specifications for Fabrication of Superconducting Cavities

International Nuclear Information System (INIS)

Antoine, C.; Foley, M.; Dhanaraj, N.

2011-01-01

It is important to distinguish among the properties of niobium, the ones that are related to the cavity's SRF performances, the formability of the material, and the mechanical behavior of the formed cavity. In general, the properties that dictate each of the above mentioned characteristics have a detrimental effect on one another and in order to preserve the superconducting properties without subduing the mechanical behavior, a balance has to be established. Depending on the applications, some parameters become less important and an understanding of the physical origin of the requirements might help in this optimization. SRF applications require high purity niobium (high RRR), but pure niobium is very soft from fabrication viewpoint. Moreover conventional fabrication techniques tend to override the effects of any metallurgical process meant to strengthen it. As those treatments dramatically affect the forming of the material they should be avoided. These unfavorable mechanical properties have to be accounted for in the design of the cavities rather than in the material specification. The aim of this paper is to review the significance of the important mechanical properties used to characterize niobium and to present the optimal range of values. Most of the following information deals with the specification of sheets for cell forming unless otherwise noted.

Physical Properties of Niobium and Specifications for Fabrication of Superconducting Cavities

Energy Technology Data Exchange (ETDEWEB)

Antoine, C.; Foley, M.; Dhanaraj, N.; /Fermilab

2011-07-01

It is important to distinguish among the properties of niobium, the ones that are related to the cavity's SRF performances, the formability of the material, and the mechanical behavior of the formed cavity. In general, the properties that dictate each of the above mentioned characteristics have a detrimental effect on one another and in order to preserve the superconducting properties without subduing the mechanical behavior, a balance has to be established. Depending on the applications, some parameters become less important and an understanding of the physical origin of the requirements might help in this optimization. SRF applications require high purity niobium (high RRR), but pure niobium is very soft from fabrication viewpoint. Moreover conventional fabrication techniques tend to override the effects of any metallurgical process meant to strengthen it. As those treatments dramatically affect the forming of the material they should be avoided. These unfavorable mechanical properties have to be accounted for in the design of the cavities rather than in the material specification. The aim of this paper is to review the significance of the important mechanical properties used to characterize niobium and to present the optimal range of values. Most of the following information deals with the specification of sheets for cell forming unless otherwise noted.

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.

Chromatographic air analyser microsystem for the selective and sensitive detection of atmospheric pollutants

International Nuclear Information System (INIS)

Sanchez, Jean-Baptiste; Lahlou, Houda; Mohsen, Yehya; Berger, Franck; Vilanova, Xavier; Correig, Xavier

2011-01-01

The development of industry and automotive trafic produces Volatile Organic Compounds (VOCs) whose toxicity can affect seriously human health and environment. The level of those contaminants in air must be as low as possible. In this context, there is a need for in situ systems that could monitor selectively the concentration of these compounds. The aim of this study is to demonstrate the efficiency of a system build with a pre-concentrator, a chromatographic micro-column and a tin oxide-based gas sensor for the selective and sensitive detection of atmospheric pollutants. In particular, this study is focused on the selective detection of benzene and 1,3 butadiene.

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

Partition/Ion-Exclusion Chromatographic Ion Stacking for the Analysis of Trace Anions in Water and Salt Samples by Ion Chromatography.

Science.gov (United States)

Akter, Fouzia; Saito, Shingo; Tasaki-Handa, Yuiko; Shibukawa, Masami

2018-01-01

A new analytical methodology for a simple and efficient on-line preconcentration of trace inorganic anions in water and salt samples prior to ion chromatographic determination is proposed. The preconcentration method is based on partition/ion-exclusion chromatographic ion stacking (PIEC ion stacking) with a hydrophilic polymer gel column containing a small amount of fixed anionic charges. The developed on-line PIEC ion stacking-ion chromatography method was validated by recovery experiments for the determination of nitrate in tap water in terms of both accuracy and precision, and the results showed the reliability of the method. The method proposed was also successfully applied to the determination of trace impurity nitrite and nitrate in reagent-grade salts of sodium sulfate. A low background level can be achieved since pure water is used as the eluant for the PIEC ion stacking. It is possible to reach sensitive detection at sub-μg L -1 levels by on-line PIEC ion stacking-ion chromatography.

Improved method for the extraction and chromatographic analysis on a fused-core column of ellagitannins found in oak-aged wine.

Science.gov (United States)

Navarro, María; Kontoudakis, Nikolaos; Canals, Joan Miquel; García-Romero, Esteban; Gómez-Alonso, Sergio; Zamora, Fernando; Hermosín-Gutiérrez, Isidro

2017-07-01

A new method for the analysis of ellagitannins observed in oak-aged wine is proposed, exhibiting interesting advantages with regard to previously reported analytical methods. The necessary extraction of ellagitannins from wine was simplified to a single step of solid phase extraction (SPE) using size exclusion chromatography with Sephadex LH-20 without the need for any previous SPE of phenolic compounds using reversed-phase materials. The quantitative recovery of wine ellagitannins requires a combined elution with methanol and ethyl acetate, especially for increasing the recovery of the less polar acutissimins. The chromatographic method was performed using a fused-core C18 column, thereby avoiding the coelution of main ellagitannins, such as vescalagin and roburin E. However, the very polar ellagitannins, namely, the roburins A, B and C, still partially coeluted, and their quantification was assisted by the MS detector. This methodology also enabled the analysis of free gallic and ellagic acids in the same chromatographic run. Copyright © 2017 Elsevier Ltd. All rights reserved.

High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

Science.gov (United States)

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

Chromatographic speciation of Cr(III)-species, inter-species equilibrium isotope fractionation and improved chemical purification strategies for high-precision isotope analysis

DEFF Research Database (Denmark)

Larsen, Kirsten Kolbjørn; Wielandt, Daniel Kim Peel; Schiller, Martin

2016-01-01

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 ...

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)

[Chromatographic mass spectrometric determination of low-molecular-weight aromatic compounds of microbial origin in the serum from patients with sepsis].

Science.gov (United States)

Beloborodova, N V; Arkhipova, A S; Beloborodov, D M; Boĭko, N B; Mel'ko, A I; Olenin, A Iu

2006-02-01

The investigation quantitatively determined the content of low-molecular-weight aromatic compounds of microbial origin in the sera of 34 individuals by chromatographic mass spectrometry. An "Agilent Technogies 6890N" gas chromatograph with a 5973 mass selective detector was applied; chromatographic separation of components was effected on an Hp-5MS quartz capillary column. Aromatic small molecules originating from microbes (SMOM) were determined in the sera of 7 patients with sepsis. The diagnosis of sepsis was documented by the presence of the systemic inflammation syndrome and by that of bacteriemia and/or artificial ventilation-associated pneumonia along with the level of procalcitonin of higher than 10 ng/ml. The levels of aromatic SMOM were compared in 10 healthy donors, 8 preoperative cardiosurgical patients, and 9 patients with different abnormalities without sepsis treated in an intensive care unit (ICU). Serum phenylacetic and 3-phenylpropionic acids were found to be prevalent in the healthy donors and postoperative cardiosurgical patients. In ICU patients with different complications without sepsis, more than half the compounds under study were undetectable, the others were found in very low concentrations, which may be accounted for by antibiotic therapy. At the same time, almost the whole spectrum of the test compounds (other than 3-phenylpropionic acid) with the highest concentrations of 3-phenyllactic, p-hydroxyphenylacetic, 3-(p-hydroxyphenyl)lactic and 2-hydroxybutanic acids, was detectable in septic patients receiving a more intensive therapy. The differences were statistically significant (by the Mann-Whitney U-test; p < 0.05). By taking into account the potentially high biological activity of the test compounds, studies are to be continued in this area.

Chemical Compositions, Chromatographic Fingerprints and Antioxidant Activities of Andrographis Herba

Directory of Open Access Journals (Sweden)

Yang Zhao

2014-11-01

Full Text Available This paper describes the development of an HPLC-UV-MS method for quantitative determination of andrographolide and dehydroandrographolide in Andrographis Herba and establishment of its chromatographic fingerprint. The method was validated for linearity, limit of detection and quantification, inter- and intra-day precisions, repeatability, stability and recovery. All the validation results of quantitative determination and fingerprinting methods were satisfactory. The developed method was then applied to assay the contents of andrographolide and dehydroandrographolide and to acquire the fingerprints of all the collected Andrographis Herba samples. Furthermore, similarity analysis and principal component analysis were used to reveal the similarities and differences between the samples on the basis of the characteristic peaks. More importantly, the DPPH free radical-scavenging and ferric reducing capacities of the Andrographis Herba samples were assayed. By bivariate correlation analysis, we found that six compounds are positively correlated to DPPH free radical scavenging and ferric reducing capacities, and four compounds are negatively correlated to DPPH free radical scavenging and ferric reducing capacities.

Volatile hexafluoroacetylacetonates for the isolation and gas-chromatographic determination of trace metals. Pt. 1

International Nuclear Information System (INIS)

Hellmuth, K.H.; Mirzai, H.

1985-01-01

The optimization of the extraction of metal cations [Sc(III), Cr(III), Mn(II), Fe(III), Co(II), Cu(II), Zn(II), Y(III), Ag(I), Cd(II), La(IIII), Ce(III), Eu(III), Yb(III), Hg(II), Pb(II), Th(IV), U(IV, VI) and Am(III)] in the form of mixed-ligand complexes with hexafluoroacetylacetone and neutral donators with nitrogen atoms or P=O-groups is described. The thermal and gas-chromatographic characteristics of the extracted volatile compounds are reported. Optimal results were achieved using tri-n-butyl-phosphine oxide as donator. (orig.) [de

INTERLABORATORY STUDY OF A THERMOSPRAY-LIQUID CHROMATOGRAPHIC/MASS SPECTROMETRIC METHOD FOR SELECTED N-METHYL CARBAMATES, N-METHYL CARBAMOYLOXIMES, AND SUBSTITUTED UREA PESTICIDES

Science.gov (United States)

A thermospray-liquid chromatographic/mass spectrometric (TS-LC/MS) method was evaluated in an interlaboratory study for determining 3 N-methyl carbamates (bendiocarb, carbaryl, and carbofuran), 3-N-methyl carbamoyloximes (aldicarb, methomyl, and oxamyl), 2 substituted urea pestic...

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.

Determination of losartan potassium, quinapril hydrochloride and hydrochlorothiazide in pharmaceutical preparations using derivative spectrophotometry and chromatographic-densitometric method.

Science.gov (United States)

Stolarczyk, Mariusz; Maślanka, Anna; Apola, Anna; Krzek, Jan

2013-01-01

Two methods, spectrophotometric and chromatographic-densitometric ones, were developed for determination of losartan potassium, quinapril hydrochloride and hydrochlorothiazide in pharmaceutical preparations. Spectrophotometric method involved derivative spectrophotometry and zero order spectrophotometry. The measurements were carried out at lambda = 224.0 nm for quinapril, lambda = 261.0 nm for hydrochlorothiazide and lambda = 270.0 nm for losartan when the derivative spectrophotometry was applied and lambda = 317.0 nm when zero order spectrophotometry was applied for the determination of hydrochlorothiazide. In chromatographic-densitometric studies high performance thin layer chromatography (HPTLC) plates were used as stationary phase and a mixture of solvents n-butanol : acetic acid : water (15 : 5 : 1, v/v/v) as mobile phase. Under the established conditions good resolution of examined constituents was obtained. Retardation factor for quinapril hydrochloride was R(f) - 0.70, for losartan potassium R(f) - 0.85 and for hydrochlorothiazide R(f) - 0.78. The developed methods are characterized by high sensitivity and accuracy. For quantitative analysis, densitometric measurements were carried out at lambda = 218.0 nm for quinapril, lambda = 275.0 nm for hydrochlorothiazide and = 232.0 nm for losartan.

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

New chromatographic method for separating Omeprazole from its degradation components and the quantitatively determining it in its pharmaceutical products

International Nuclear Information System (INIS)

Touma, M.; Rajab, A.; Seuleiman, M.

2007-01-01

New chromatographic method for Quantitative Determination of Omeprazole in its Pharmaceutical Products was produced. Omeprazole and its degradation components were well separated in same chromatogram by using high perfume liquid chromatography (HPLC). The new analytical method has been validated by these characteristic tests (accuracy, precision, range, linearity, specificity/selectivity, limit of detection (LOD) and limit of quantitative (LOQ) ).(author)

New chromatographic Methods for Separation of Lansoprazole from its Degradation Components and The Quantitative Determination in its Pharmaceutical Products

International Nuclear Information System (INIS)

Touma, M.; Rajab, A.

2009-01-01

New chromatographic method was found for Quantitative Determination of Lansoprazole in its pharmaceutical products. Lansoprazole and its degradation components were well separated in same chromatogram by using high perfume liquid chromatography (HPLC). The new analytical method has been validated by these characteristic tests (accuracy, precision, range, linearity, specificity/selectivity, limit of detection (LOD) and limit of quantitative (LOQ)). (author)

Radio Column Chromatographic Assay of H3-Labelled Substances

International Nuclear Information System (INIS)

Scharpenseel, H.W.; Menke, K.H.

1962-01-01

Combined radio-chromatographic investigations of H 3 -labelled substances are an integral part of the majority of biochemical experiments with H 3 -labelled compounds. H 3 -radio paper chromatography yields, in a scanner with a windowless flow counter, a counting efficiency of 0,5 -1,5%, depending largely on the thickness of the paper and the self-absorption of the labelled compound. The radio gas chromatography of tritiated compounds presents no major problem. Successful use is being made of a combination of a gas chromatograph with a flow ionization chamber and vibrating reed electrometer, a system originated by K. E. Wilzbach and P. Riessz, and improved by H. Dutton, L. Mason and L. Blair. Through the use of ''Teflon'' and silicone-rubber for the insulating parts of the flow ion chamber, it can be operated at close to 300 o C. Radio column chromatography with tritium holds little promise, when the column effluent is spread out as a shallow layer and slowly passes under a windowless flow counter or a scintillation counter, as was successfully tried with C 14 . Liquid scintillation spectrometry is likely to be the chosen method. Essentially, there are two different approaches feasible. These have been compared: 1. The column effluent is passed through a coil of plastic scintillator tubing, which is wound around a ''Plexiglas'' cylinder and placed in a bath of silicone oil in a light pipe with TiO 2 -reflector. Similarly, the HP-containing effluent can be directed through a test vial, filled - very much as in Steinberg's method - with plastic scintillator beads. These two approaches, that operate highly satisfactorily in the case of C 14 , offer low counting efficiencies of less than 1% for H 3 due to the unfavourable surface to volume ratio. 2. The column effluent is combined 1:30 with a mixture of 3:2 toluene/ethanol by the action of a magnet-vibrator before being assayed while passing through a K 40 -free glass - coiled between the analyser- and monitor

Domestic Preparedness Program: Evaluation of the Agilent Gas Chromatograph - Flame Photometric Detector/Mass Selective Detector (GC-FPD/MSD) System Against Chemical Warfare Agents Summary Report

National Research Council Canada - National Science Library

Longworth, Terri

2003-01-01

This report characterizes the chemical warfare agent (CWA) detection potential of the commercially available Agilent gas chromatograph-flame photometric detector/mass selective detector (GC-FPD/MSD...

Equations for nickel-chromium wire heaters of column transfer lines in gas chromatographic-electroantennographic detection (GC-EAD).

Science.gov (United States)

Byers, John A

2004-05-30

Heating of chromatographic columns, transfer lines, and other devices is often required in neuroscience research. For example, volatile compounds passing through a capillary column of a gas chromatograph (GC) can be split, with half exiting the instrument through a heated transfer line to an insect antenna or olfactory sensillum for electroantennographic detector (GC-EAD) recordings. The heated transfer line is used to prevent condensation of various chemicals in the capillary that would otherwise occur at room temperature. Construction of such a transfer line heater is described using (80/20%) nickel-chromium heating wire wrapped in a helical coil and powered by a 120/220 V ac rheostat. Algorithms were developed in a computer program to estimate the voltage at which a rheostat should be set to obtain the desired heater temperature for a specific coil. The coil attributes (radius, width, number of loops, or length of each loop) are input by the user, as well as AWG size of heating wire and desired heater temperature. The program calculates total length of wire in the helix, resistance of the wire, amperage used, and the voltage to set the rheostat. A discussion of semiochemical isolation methods using the GC-EAD and bioassays is presented.

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.

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.

Comparison of structure and organization of cutaneous lipids in a reconstructed skin model and human skin: spectroscopic imaging and chromatographic profiling.

Science.gov (United States)

Tfayli, Ali; Bonnier, Franck; Farhane, Zeineb; Libong, Danielle; Byrne, Hugh J; Baillet-Guffroy, Arlette

2014-06-01

The use of animals for scientific research is increasingly restricted by legislation, increasing the demand for human skin models. These constructs present comparable bulk lipid content to human skin. However, their permeability is significantly higher, limiting their applicability as models of barrier function, although the molecular origins of this reduced barrier function remain unclear. This study analyses the stratum corneum (SC) of one such commercially available reconstructed skin model (RSM) compared with human SC by spectroscopic imaging and chromatographic profiling. Total lipid composition was compared by chromatographic analysis (HPLC). Raman spectroscopy was used to evaluate the conformational order, lateral packing and distribution of lipids in the surface and skin/RSM sections. Although HPLC indicates that all SC lipid classes are present, significant differences are observed in ceramide profiles. Raman imaging demonstrated that the RSM lipids are distributed in a non-continuous matrix, providing a better understanding of the limited barrier function. © 2014 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

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

The World Health Organization accepts chromatographic fingerprints as a tool for identification and quality control of herbal medicines. This is the first study in which the distinction, identification and quality control of four different Artemisia species, i.e. Artemisia vulgaris, A. absinthium, A. annua and A. capillaris samples, is performed based on the evaluation of entire chromatographic fingerprint profiles developed with identical experimental conditions. High-Performance Liquid Chromatography (HPLC) with Diode Array Detection (DAD) was used to develop the fingerprints. Application of factorial designs leads to methanol/water (80:20 (v/v)) as the best extraction solvent for the pulverised plant material and to a shaking bath for 30 min as extraction method. Further, so-called screening, optimisation and fine-tuning phases were performed during fingerprint development. Most information about the different Artemisia species, i.e. the highest number of separated peaks in the fingerprint, was acquired on four coupled Chromolith columns (100 mm × 4.6 mm I.D.). Trifluoroacetic acid 0.05% (v/v) was used as mobile-phase additive in a stepwise linear methanol/water gradient, i.e. 5, 34, 41, 72 and 95% (v/v) methanol at 0, 9, 30, 44 and 51 min, where the last mobile phase composition was kept isocratic till 60 min. One detection wavelength was selected to perform data analysis. The lowest similarity between the fingerprints of the four species was present at 214 nm. The HPLC/DAD method was applied on 199 herbal samples of the four Artemisia species, resulting in 357 fingerprints. The within- and between-day variation of the entire method, as well as the quality control fingerprints obtained during routine analysis, were found acceptable. The distinction of these Artemisia species was evaluated based on the entire chromatographic profiles, developed by a shared method, and visualised in score plots by means of the Principal Component Analysis (PCA) exploratory data

Gel chromatographic behavior of Tc-99m-labeled compounds in aqueous solution

International Nuclear Information System (INIS)

Suzuki, T.; Wagner, H.N. Jr.; Burns, H.D.; Dannals, F.F.

1984-01-01

The purpose of this study was to elucidate the interaction of Tc-99m-labeled compounds (Tc-99m 0/sub 4/-bar, Tc-99m glucoheptonate, Tc-99m DTPA, Tc-99m disofenin) with the chromatographic gels, to determine their relative molecular sizes and molecular structures in aqueous solution, which are based on their biomenbrane transport mechanism and quality control analysis. Each Tc-99m-labeled compound was eluted and analyzed by three different gel chromatrography systems varying buffers: Sephadex G-25, Sephadex LH-20 and Bio-Gel P-4. The best separation between the elution peaks of all compounds except Tc-99m glucoheptonate was achieved on Sephadex G-25 in methanol-0.025OM Tris-HCL buffer (pH 7.6) (1:1) which could avoid the aromatic interaction with the gels. Tc-99m glucoheptonate was well eluted only on a Bio-Gel P-4 column but its elution peak was not separated from other compounds' peaks. The elution of Tc-99m disofenin was delayed on Sephadex G-25 gel and Bio-Gel P-4 columns in 0.9% NaCl and Tris-HCl buffer(ph 7.6) and on Sephadex LH-20 column in methanol-Tris-HCl buffer, because of the aromatic ring interaction with the gels. The relative molecular size index ( Kav ) calculated from the elution volume of the gel chromatography. Kav of Tc-99m 0/sub 4/-bar(MW=163), Tc-99m DTPA (MW=492?) and TC-99m disofenin (MW=707) on Sephadex G-25 in methanol-0.025OM Tris-HCl buffer(pH 7.6) (1:1), which was the most suitable combination of the gel and the buffer, were 0.976, 0.477 and 0.200, respectively. They inversely correlated with their estimated molecular weight. The interaction of Tc-99m-labeled compounds with the chromatographic gels should be considered in quality control procedure for Tc-99m radiopharamaceuticals

Automated optimization and construction of chemometric models based on highly variable raw chromatographic data.

Science.gov (United States)

Sinkov, Nikolai A; Johnston, Brandon M; Sandercock, P Mark L; Harynuk, James J

2011-07-04

Direct chemometric interpretation of raw chromatographic data (as opposed to integrated peak tables) has been shown to be advantageous in many circumstances. However, this approach presents two significant challenges: data alignment and feature selection. In order to interpret the data, the time axes must be precisely aligned so that the signal from each analyte is recorded at the same coordinates in the data matrix for each and every analyzed sample. Several alignment approaches exist in the literature and they work well when the samples being aligned are reasonably similar. In cases where the background matrix for a series of samples to be modeled is highly variable, the performance of these approaches suffers. Considering the challenge of feature selection, when the raw data are used each signal at each time is viewed as an individual, independent variable; with the data rates of modern chromatographic systems, this generates hundreds of thousands of candidate variables, or tens of millions of candidate variables if multivariate detectors such as mass spectrometers are utilized. Consequently, an automated approach to identify and select appropriate variables for inclusion in a model is desirable. In this research we present an alignment approach that relies on a series of deuterated alkanes which act as retention anchors for an alignment signal, and couple this with an automated feature selection routine based on our novel cluster resolution metric for the construction of a chemometric model. The model system that we use to demonstrate these approaches is a series of simulated arson debris samples analyzed by passive headspace extraction, GC-MS, and interpreted using partial least squares discriminant analysis (PLS-DA). Copyright © 2011 Elsevier B.V. All rights reserved.

Stonin 2 Overexpression is Correlated with Unfavorable Prognosis and Tumor Invasion in Epithelial Ovarian Cancer

Directory of Open Access Journals (Sweden)

Xiaoying Sun

2017-07-01

Full Text Available Stonin 2 (STON2, which functions in adjusting endocytotic complexes, is probably involved in the monitoring of the internalization of dopamine D2 receptors which have an inhibitory action of dopamine on tumor progression. However, its clinical significance in tumor progression and prognosis remains unclear. We explored the association between STON2 and the clinicopathological characteristics of epithelial ovarian cancer (EOC. The STON2 levels in ovarian cancer and normal cell lines and tissues were detected by real-time PCR and Western blot analyses. STON2 protein expression was also detected by an immunohistochemical analysis. The clinical significance of STON2 expression in ovarian cancer was statistically analyzed. STON2 significantly increased in the ovarian cancer cell lines and tissues compared to the normal ones. In the 89 EOC samples tested, STON2 expression was significantly correlated with intraperitoneal metastasis, intestinal metastasis, intraperitoneal recurrence, ascites containing tumor cells, and CA153 level. Moreover, patients with STON2 protein overexpression were more likely to exhibit platinum resistance and to have undergone neoadjuvant chemotherapy. Patients with high STON2 protein expression had a tendency to have a shorter overall survival and a poor prognosis. A multivariate analysis showed that STON2 was an independent prognostic predictor for EOC patients. In conclusion, STON2 plays an important role in the progression and prognosis of ovarian carcinoma, especially in platinum resistance, intraperitoneal metastasis, and recurrence. STON2 can be a novel antitumor drug target and biomarker which predicts an unfavorable prognosis for EOC patients.

Tobacco Smoking During Radiation Therapy for Head-and-Neck Cancer Is Associated With Unfavorable Outcome

International Nuclear Information System (INIS)

Chen, Allen M.; Chen, Leon M.; Vaughan, Andrew; Sreeraman, Radhika; Farwell, D. Gregory; Luu, Quang; Lau, Derick H.; Stuart, Kerri; Purdy, James A.; Vijayakumar, Srinivasan

2011-01-01

Purpose: To evaluate the effect of continued cigarette smoking among patients undergoing radiation therapy for head-and-neck cancer by comparing the clinical outcomes among active smokers and quitters. Methods and Materials: A review of medical records identified 101 patients with newly diagnosed squamous cell carcinoma of the head and neck who continued to smoke during radiation therapy. Each active smoker was matched to a control patient who had quit smoking before initiation of radiation therapy. Matching was based on tobacco history (pack-years), primary site, age, sex, Karnofsky Performance Status, disease stage, radiation dose, chemotherapy use, year of treatment, and whether surgical resection was performed. Outcomes were compared by use of Kaplan-Meier analysis. Normal tissue effects were graded according to the Radiation Therapy Oncology Group/European Organization for the Treatment of Cancer toxicity criteria. Results: With a median follow-up of 49 months, active smokers had significantly inferior 5-year overall survival (23% vs. 55%), locoregional control (58% vs. 69%), and disease-free survival (42% vs. 65%) compared with the former smokers who had quit before radiation therapy (p < 0.05 for all). These differences remained statistically significant when patients treated by postoperative or definitive radiation therapy were analyzed separately. The incidence of Grade 3 or greater late complications was also significantly increased among active smokers compared with former smokers (49% vs. 31%, p = 0.01). Conclusions: Tobacco smoking during radiation therapy for head-and-neck cancer is associated with unfavorable outcomes. Further studies analyzing the biologic and molecular reasons underlying these differences are planned.

Diagnosis of rinderpest in Tanzania by a rapid chromatographic strip-test.

Science.gov (United States)

Wambura, P N; Moshy, D W; Mbise, A N; Mollel, G O; Taylor, W P; Anderson, J; Bruning, A

2000-06-01

A simple chromatographic strip-test based on Clearview technology, is under development as a pen-side test for the detection of rinderpest antigen in eye swabs taken from cattle in the field. An outbreak of rinderpest occurred in the northern zone of Tanzania from late February to June 1997. The affected cattle exhibited very mild clinical signs, which made clinical diagnosis difficult. One hundred and seven eye swabs were collected from cattle suspected of infection with rinderpest. These were tested in the field using a prototype of the pen-side test and 13 (12.15%) of the samples were found to be positive for the presence of rinderpest antigen. These were confirmed by ICE. The positive cases were predominantly found in the Ngorongoro district. This demonstrates the usefulness of such a simple, rapid pen-side diagnostic assay, particularly when clinically 'mild' strains of rinderpest are present.

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.

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.

Chromatographic, Spectrometric and NMR Characterization of a New Set of Glucuronic Acid Esters Synthesized by Lipase

Directory of Open Access Journals (Sweden)

Michel Marlier

2007-01-01

Full Text Available An enzymatic synthesis was developed on a new set of D-glucuronic acid esters and particularly the tetradecyl-D-glucopyranosiduronate also named tetradecyl D-glucuronate. Chromatographic analyses revealed the presence of the ester as a mixture of anomeric forms for carbon chain lengths superior to 12. TOF/MS and MS/MS studies confirmed the synthesis of glucuronic acid ester. The NMR study also confirmed the structure of glucuronic acid esters and clearly revealed an anomeric (α/β ratio equivalent to 3/2

Batch-to-Batch Quality Consistency Evaluation of Botanical Drug Products Using Multivariate Statistical Analysis of the Chromatographic Fingerprint

OpenAIRE

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

2013-01-01

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 ...

Chiral high-performance liquid chromatographic analysis of fluoxetine and norfluoxetine in rabbit plasma, urine, and vitreous humor using an acetylated beta-cyclodextrin column.

Science.gov (United States)

Yee, L; Wong, S H; Skrinska, V A

2000-10-01

Fluoxetine (Prozac) is a potent selective serotonin reuptake inhibitor used for the treatment of major depression. Both fluoxetine (F) and its demethylated metabolite, norfluoxetine (NF), are racemic. S-Fluoxetine (SF) and S-norfluoxetine (SNF) are more potent inhibitors of serotonin reuptake than R-fluoxetine (RF) and R-norfluoxetine (RNF). Quantitation of individual enantiomers may provide a greater understanding of pharmacokinetic properties. The objective of this study was to perform a limited chiral selectivity study using rabbit plasma, urine, and vitreous humor analyzed by a solid-phase extraction protocol and a newly developed chiral analysis with an acetylated beta-cyclodextrin (CD) column. Liquid chromatographic parameters for CD were as follows: a mobile phase composition of methanol/0.3% triethylamine buffer, pH 5.6, (30:70), a flow rate of 1 mL/min, detection at 214 nm, and a temperature of 40 degrees C. Elution order was SNF, SF, RNF, and RF with capacity factors of 6, 7, 8, and 9, respectively. The corresponding resolution factors were as follows: R1,2 = 0.8, R2,3 = 1.2, and R3,4 = 0.9. The conditions for solid-phase extraction were optimized for Varian Bond Elut Certify columns. Following sample application, the column was rinsed with water, acetic acid, and then with methanol. Drug enantiomers were eluted with methylene chloride, isopropanol, and ammonium hydroxide (78:20:2). After extract evaporation, the extract residue was reconstituted for high-performance liquid chromatographic analysis. To investigate chiral pharmacology, a biodistribution study was performed by administering 2 mg/kg of F to five rabbits. Blood, urine, and vitreous specimens were collected. Plasma samples collected 45 min postinjection showed nearly equal concentrations of RF and SE After 24 h, the only metabolite detected in plasma was RNF. Drugs were not detectable in vitreous humor. Urine concentrations of SNF, SF, RNF, and RF were 51, 76, 34, and 8 microg/L, respectively

Extractability of water-soluble soil organic matter as monitored by spectroscopic and chromatographic analyses.

Science.gov (United States)

Nkhili, Ezzhora; Guyot, Ghislain; Vassal, Nathalie; Richard, Claire

2012-07-01

Cold and hot water processes have been intensively used to recover soil organic matter, but the effect of extraction conditions on the composition of the extracts were not well investigated. Our objective was to optimize the extraction conditions (time and temperature) to increase the extracted carbon efficiency while minimizing the possible alteration of water extractable organic matter of soil (WEOM). WEOM were extracted at 20°C, 60°C, or 80°C for 24 h, 10-60 min, and 20 min, respectively. The different processes were compared in terms of pH of suspensions, yield of organic carbon, spectroscopic properties (ultraviolet-visible absorption and fluorescence), and by chromatographic analyses. For extraction at 60°C, the time 30 min was optimal in terms of yield of organic carbon extracted and concentration of absorbing and fluorescent species. The comparison of WEOM 20°C, 24 h; 60°C, 30 min; and 80°C, 20 min highlighted significant differences. The content of total organic carbon, the value of specific ultraviolet absorbance (SUVA(254)), the absorbance ratio at 254 and 365 nm (E (2)/E (3)), and the humification index varied in the order: WEOM (20°C, 24 h) < WEOM (80°C, 20 min) < WEOM (60°C, 30 min). The three WEOM contained common fluorophores associated with simple aromatic structures and/or fulvic-like and common peaks of distinct polarity as detected by ultra performance liquid chromatography. For the soil chosen, extraction at 60°C for 30 min is the best procedure for enrichment in organic chemicals and minimal alteration of the organic matter.

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

Obese Patients With a Binge Eating Disorder Have an Unfavorable Metabolic and Inflammatory Profile.

Science.gov (United States)

Succurro, Elena; Segura-Garcia, Cristina; Ruffo, Mariafrancesca; Caroleo, Mariarita; Rania, Marianna; Aloi, Matteo; De Fazio, Pasquale; Sesti, Giorgio; Arturi, Franco

2015-12-01

To evaluate whether obese patients with a binge eating disorder (BED) have an altered metabolic and inflammatory profile related to their eating behaviors compared with non-BED obese.A total of 115 White obese patients consecutively recruited underwent biochemical, anthropometrical evaluation, and a 75-g oral glucose tolerance test. Patients answered the Binge Eating Scale and were interviewed by a psychiatrist. The patients were subsequently divided into 2 groups according to diagnosis: non-BED obese (n = 85) and BED obese (n = 30). Structural equation modeling analysis was performed to elucidate the relation between eating behaviors and metabolic and inflammatory profile.BED obese exhibited significantly higher percentages of altered eating behaviors, body mass index (P < 0.001), waist circumference (P < 0.01), fat mass (P < 0.001), and a lower lean mass (P < 0.001) when compared with non-BED obese. Binge eating disorder obese also had a worse metabolic and inflammatory profile, exhibiting significantly lower high-density lipoprotein cholesterol levels (P < 0.05), and higher levels of glycated hemoglobin (P < 0.01), uric acid (P < 0.05), erythrocyte sedimentation rate (P < 0.001), high-sensitive C-reactive protein (P < 0.01), and white blood cell counts (P < 0.01). Higher fasting insulin (P < 0.01) and higher insulin resistance (P < 0.01), assessed by homeostasis model assessment index and visceral adiposity index (P < 0.001), were observed among BED obese. All differences remained significant after adjusting for body mass index. No significant differences in fasting plasma glucose or 2-hour postchallenge plasma glucose were found. Structural equation modeling analysis confirmed the relation between the altered eating behaviors of BED and the metabolic and inflammatory profile.Binge eating disorder obese exhibited an unfavorable metabolic and inflammatory profile, which is related to their characteristic

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.

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).

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.

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).

Liquid Chromatographic-Chemometric Techniques for the Simultaneous HPLC Determination of Lansoprazole, Amoxicillin and Clarithromycin in Commercial Preparation.

Science.gov (United States)

Aktas, A Hakan; Saridag, Ayse Mine

2017-09-01

Two multivariate calibration-prediction techniques, principal component regression (PCR) and partial least-squares regression (PLSR) were applied to the chromatographic multicomponent analysis of the drug containing lansoprazole (LAN), clarithromycin (CLA) and amoxicillin (AMO). Optimum chromatographic separation of LAN, CLA and AMO with atorvastatin as the internal standard (IS) was obtained by using Xterra® RP18 column 5 μm 4.6 × 250 mm2, and 25 mM ammonium chloride buffer prepared ammonium chloride, acetonitrile and bidistilled water (45:45:10 v/v) as the mobile phase at flow rate 1.0 mL/min. The high pressure liquid chromatography data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using diode array detector detection at five wavelengths (205, 210, 215, 220 and 225 nm). LC-chemometric calibration for LAN, CLA and AMO were separately constructed by using the relationship between the peak-area ratio and training sets for each analyte. A series of synthetic solutions containing different concentrations of LAN, CLA and AMO were used to check the prediction ability of the PCR and PLS. Both of the two-chemometric methods in this study can be satisfactorily used for the quantitative analysis and for dissolutions tests of multicomponent commercial drug. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

Science.gov (United States)

MacAskill, John A.; Tsikata, Edem

2014-01-01

We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

Extraction chromatographic method of uranium(VI) with high molecular mass amine (ALIQUAT - 336)

International Nuclear Information System (INIS)

Roy, Uday Sankar; Dutta, Keshab Kumar

1999-01-01

A selective method has been developed for reversed phase extraction chromatographic studies of uranium(VI) with Aliquat - 336 (liquid anion exchanger) coated on silica gel as stationary phase. Quantitative extraction of uranium has been achieved in HCl - medium from 1.25(M)-4(M). The effect of different acids with various concentrations stripping agents, flow rate on extraction and elution have been investigated. The exchange capacity of the prepared exchanger has been determined. Uranium(VI) has been separated quantitatively from Th, Ce, Zr, Pb, Ga, Hg, Fe, La, Pr, Nd, Sm and Cr from a binary mixture by controlling the extraction and elution conditions. The separation of U(VI) from ternary and quarternary mixtures of various metal ions has also been achieved. (author)

Chromatographic cation exchange separation of decigram quantities of californium and other transplutonium elements

Energy Technology Data Exchange (ETDEWEB)

Benker, D.E.; Chattin, F.R.; Collins, E.D.; Knauer, J.B.; Orr, P.B.; Ross, R.G.; Wiggins, J.T.

1980-01-01

Decigram quantities of highly radioactive transplutonium elements are routinely partitioned at TRU by chromatographic elution from cation resin using AHIB eluent. By using two high-pressure ion exchange columns, a small one for the initial loading of the feed and a large one for the elution, batch runs containing up to 200 mg of /sup 252/Cf can be made in about 5 hours (2 hours to load the feed and 3 hours for the elution). The number of effluent product fractions and the amount of actinides that must be collected in intermediate fractions are minimized by monitoring response from a flow-through alpha-detector. This process has been reliable and relatively easy to operate, and will continue to be used for partitioning transplutonium elements at TRU.

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

The separation of sup(99m)Tc from 99Mo through an aluminium oxide chromatographic columm

International Nuclear Information System (INIS)

Imoto, S.T.

1980-01-01

The separation of sup(99m)Tc from 99 Mo using the chromatographic method is studied. Alumina is used as adsorbent. The pH values for adsorption of carrier-free 99 Mo on columns filled with ordinary alumina and with that thermically treated at 1000 0 C for five hours, and the separation conditions of sup(99m)Tc using physiologic solution as eluent are determined. The sup(99m)Tc separation yields of both columns are compared and the quality of the products obtained by successive elutions for 10 days is analyzed. (Author) [pt

Optimization of the reversed-phase high-performance liquid chromatographic separation of synthetic estrogenic and progestogenic steroids using the multi-criteria decision making method

NARCIS (Netherlands)

Smilde, A. K.; Bruins, C. H.; Doornbos, D. A.; Vink, J.

1987-01-01

The optimization of the reversed-phase high-performance liquid chromatographic separation of a mixture of ethynylestradiol, desogestrel and three related compounds is described. A procedure is used that allows the prediction of the capacity factors of each individual synthetic steroid, depending on

Chitosan fibers with improved biological and mechanical properties for tissue engineering applications.

Science.gov (United States)

Albanna, Mohammad Z; Bou-Akl, Therese H; Blowytsky, Oksana; Walters, Henry L; Matthew, Howard W T

2013-04-01

The low mechanical properties of hydrogel materials such as chitosan hinder their broad utility for tissue engineering applications. Previous research efforts improved the mechanical properties of chitosan fiber through chemical and physical modifications; however, unfavorable toxicity effects on cells were reported. In this paper, we report the preparation of chitosan fibers with improved mechanical and biocompatibility properties. The structure-property relationships of extruded chitosan fibers were explored by varying acetic acid (AA) concentration, ammonia concentration, annealing temperature and degree of heparin crosslinking. Results showed that optimizing AA concentration to 2vol% improved fiber strength and stiffness by 2-fold. Extruding chitosan solution into 25wt% of ammonia solution reduced fiber diameters and improved fiber strength by 2-fold and stiffness by 3-fold, due to an increase in crystallinity as confirmed by XRD. Fiber annealing further reduced fiber diameter and improved fiber strength and stiffness as temperature increased. Chitosan fibers crosslinked with heparin had increased diameter but lower strength and stiffness properties and higher breaking strain values. When individual parameters were combined, further improvement in fiber mechanical properties was achieved. All mechanically improved fibers and heparin crosslinked fibers promoted valvular interstitial cells (VIC) attachment and growth over 10 day cultures. Our results demonstrate the ability to substantially improve the mechanical properties of chitosan fibers without adversely affecting their biological properties. The investigated treatments offer numerous advantages over previous physical/chemical modifications and thus are expected to expand the utility of chitosan fibers with tunable mechanical properties in various tissue engineering applications. Copyright © 2012 Elsevier Ltd. All rights reserved.

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

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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.

Physical properties and structure of fine core-shell particles used as packing materials for chromatography Relationships between particle characteristics and column performance.

Science.gov (United States)

Gritti, Fabrice; Leonardis, Irene; Abia, Jude; Guiochon, Georges

2010-06-11

The recent development of new brands of packing materials made of fine porous-shell particles, e.g., Halo and Kinetex, has brought great improvements in potential column efficiency, demanding considerable progress in the design of chromatographic instruments. Columns packed with Halo and Kinetex particles provide minimum values of their reduced plate heights of nearly 1.5 and 1.2, respectively. These packing materials have physical properties that set them apart from conventional porous particles. The kinetic performance of 4.6mm I.D. columns packed with these two new materials is analyzed based on the results of a series of nine independent and complementary experiments: low-temperature nitrogen adsorption (LTNA), scanning electron microscopy (SEM), inverse size-exclusion chromatography (ISEC), Coulter counter particle size distributions, pycnometry, height equivalent to a theoretical plate (HETP), peak parking method (PP), total pore blocking method (TPB), and local electrochemical detection across the column exit section (LED). The results of this work establish links between the physical properties of these superficially porous particles and the excellent kinetic performance of columns packed with them. It clarifies the fundamental origin of the difference in the chromatographic performances of the Halo and the Kinetex columns. Copyright 2010 Elsevier B.V. All rights reserved.

High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010 on cellulose ramification chiral stationary phase

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Ying Zhou

2012-02-01

Full Text Available The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ by high performance liquid chromatographic (HPLC methods, which included ibuprofen (C1, ketoprofen (C2, nitrendipine (C3, nimodipine (C4, felodipine (C5, omeprazole (C6, praziquantel (C7, propranolol hydrochloride (C8, atenolol (C9, sulpiride (C10, clenbuterol hydrochloride (C11, verapamil hydrochloride (C12, and chlorphenamine maleate (C13. The mobile phase consisted of isopropanol and n-hexane. The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min. The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied, while the effects of proportion of organic additives, alcohol displacer and temperature on the separation were studied. And the mechanism of some of racemates was discussed. The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When concentration of organic alkaline modifier was 0.2% (v/v, the resolution and the peak shape were fairly good. Most racemates mentioned above had better resolution at column temperature of 25 °C. When racemates were separated, the temperature should be kept so as to obtain stable separation results. Keywords: HPLC, Chiral stationary phase, Optical enantiomers, Cellulose ramification

On the ability of the Viking gas chromatograph-mass spectrometer to detect organic matter.

Science.gov (United States)

Biemann, Klaus

2007-06-19

A recent paper by Navarro-Gonzalez et al. [Navarro-Gonzalez R, Navarro KF, de la Rosa J, Iniguez E, Molina P, Miranda LD, Morales P, Cienfuegos E, Coll P, Raulin F, et al. (2006) Proc Natl Acad Sci USA 103:16089-16094] claims to show that the Viking GCMS (gas chromatograph-mass spectrometer) experiment, which carried out a search for organic matter at the surface of Mars in 1976, "may have been blind to low levels of organics." To rebut this assertion, the Viking experiment, test data, and results on Mars are reviewed, and the fallacies in the design, execution, and interpretation of the new experiments presented by Navarro-Gonzalez et al. are critically examined.

Gas-chromatographic separation of hydrogen isotopes mixtures on capillary molecular sieve 5 A column at 173 K

International Nuclear Information System (INIS)

Bidica, N.; Preda, A.; Stanciu, V.

2002-01-01

Analysis of a gas mixture of hydrogen species, is not too easy because the differences in their physical-chemical properties are very small; the most different are their masses, and consequently most common analytical method appear to be the mass-spectrometry. However, the impossibility to distinguish between two ions (atomic or molecular) with the same mass renders this method as unapplicable. Another problem is the decay of tritium with production of 3 He. These disadvantages of mass-spectrometry have made that other analytical methods, like gas chromatography, to be considered and developed. Thus, there are many papers about various chromatographic columns especially prepared for hydrogen species separation but the preparation and treatment of these columns are very difficult to reproduce. Besides these, there are two other main disadvantages: column operating temperature is very low and long retention times for hydrogen species (more than half an hour) are required. However, the gas-chromatography method still remains an appropriate one. The method described in this paper was based on using a capillary molecular sieve 5A column which has been operated for this kind of separation. The retention times were relatively short, about 8-9 minutes. The carrier gas was Ne and the detector - TCD. In the paper chromatograms for various carrier flow rates and various hydrogen isotope mixtures are presented. The results demonstrated a quite good efficiency for H 2 , HD, D 2 and a not very good one for orthoH 2 -paraH 2 . (authors)

Effect of preconditioning cobalt and nickel based dental alloys with Bacillus sp. extract on their surface physicochemical properties and theoretical prediction of Candida albicans adhesion

International Nuclear Information System (INIS)

Balouiri, Mounyr; Bouhdid, Samira; Sadiki, Moulay; Ouedrhiri, Wessal; Barkai, Hassan; El Farricha, Omar; Ibnsouda, Saad Koraichi; Harki, El Houssaine

2017-01-01

Biofilm formation on dental biomaterials is implicated in various oral health problems. Thus the challenge is to prevent the formation of this consortium of microorganisms using a safe approach such as antimicrobial and anti-adhesive natural products. Indeed, in the present study, the effects of an antifungal extract of Bacillus sp., isolated from plant rhizosphere, on the surface physicochemical properties of cobalt and nickel based dental alloys were studied using the contact angle measurements. Furthermore, in order to predict the adhesion of Candida albicans to the treated and untreated dental alloys, the total free energy of adhesion was calculated based on the extended Derjaguin-Landau-Verwey-Overbeek approach. Results showed hydrophobic and weak electron-donor and electron-acceptor characteristics of both untreated dental alloys. After treatment with the antifungal extract, the surface free energy of both dental alloys was influenced significantly, mostly for cobalt based alloy. In fact, treated cobalt based alloy became hydrophilic and predominantly electron donating. Those effects were time-dependent. Consequently, the total free energy of adhesion of C. albicans to this alloy became unfavorable after treatment with the investigated microbial extract. A linear relationship between the electron-donor property and the total free energy of adhesion has been found for both dental alloys. Also, a linear relationship has been found between this latter and the hydrophobicity for the cobalt based alloy. However, the exposure of nickel based alloy to the antifungal extract failed to produce the same effect. - Highlights: • Assessment of dental alloys physicochemical properties using contact angle method • Evaluation for the first time of microbial coating impact on dental alloys surface • Decrease of hydrophobicity of treated cobalt-chromium alloy with antifungal extract • Increase of Lewis base property of treated cobalt-chromium with treatment �

Effect of preconditioning cobalt and nickel based dental alloys with Bacillus sp. extract on their surface physicochemical properties and theoretical prediction of Candida albicans adhesion

Energy Technology Data Exchange (ETDEWEB)

Balouiri, Mounyr, E-mail: b.mounyr@gmail.com [Faculté des Sciences et Techniques, Université Sidi Mohamed Ben Abdellah, BP 2202, 30007 Fez (Morocco); Bouhdid, Samira [Faculté des Sciences de Tétouan, Université Abdelmalek Essaadi, Avenue de Sebta, Mhannech II, 93002 Tétouan (Morocco); Sadiki, Moulay; Ouedrhiri, Wessal; Barkai, Hassan; El Farricha, Omar [Faculté des Sciences et Techniques, Université Sidi Mohamed Ben Abdellah, BP 2202, 30007 Fez (Morocco); Ibnsouda, Saad Koraichi [Faculté des Sciences et Techniques, Université Sidi Mohamed Ben Abdellah, BP 2202, 30007 Fez (Morocco); Cité de l' innovation, Université Sidi Mohamed Ben Abdellah, BP 2626, 30007 Fez (Morocco); Harki, El Houssaine [Faculté des Sciences et Techniques, Université Sidi Mohamed Ben Abdellah, BP 2202, 30007 Fez (Morocco)

2017-02-01

Biofilm formation on dental biomaterials is implicated in various oral health problems. Thus the challenge is to prevent the formation of this consortium of microorganisms using a safe approach such as antimicrobial and anti-adhesive natural products. Indeed, in the present study, the effects of an antifungal extract of Bacillus sp., isolated from plant rhizosphere, on the surface physicochemical properties of cobalt and nickel based dental alloys were studied using the contact angle measurements. Furthermore, in order to predict the adhesion of Candida albicans to the treated and untreated dental alloys, the total free energy of adhesion was calculated based on the extended Derjaguin-Landau-Verwey-Overbeek approach. Results showed hydrophobic and weak electron-donor and electron-acceptor characteristics of both untreated dental alloys. After treatment with the antifungal extract, the surface free energy of both dental alloys was influenced significantly, mostly for cobalt based alloy. In fact, treated cobalt based alloy became hydrophilic and predominantly electron donating. Those effects were time-dependent. Consequently, the total free energy of adhesion of C. albicans to this alloy became unfavorable after treatment with the investigated microbial extract. A linear relationship between the electron-donor property and the total free energy of adhesion has been found for both dental alloys. Also, a linear relationship has been found between this latter and the hydrophobicity for the cobalt based alloy. However, the exposure of nickel based alloy to the antifungal extract failed to produce the same effect. - Highlights: • Assessment of dental alloys physicochemical properties using contact angle method • Evaluation for the first time of microbial coating impact on dental alloys surface • Decrease of hydrophobicity of treated cobalt-chromium alloy with antifungal extract • Increase of Lewis base property of treated cobalt-chromium with treatment �

Interim report of image-guided conformal high-dose-rate brachytherapy for patients with unfavorable prostate cancer: the William Beaumont Phase II dose-escalating trial

International Nuclear Information System (INIS)

Martinez, Alvaro A.; Kestin, Larry L.; Stromberg, Jannifer S.; Gonzalez, Jose A.; Wallace, Michelle; Gustafson, Gary S.; Edmundson, Gregory K.; Spencer, William; Vicini, Frank A.

2000-01-01

Purpose: We analyzed our institution's experience treating patients with unfavorable prostate cancer in a prospective Phase II dose-escalating trial of external beam radiation therapy (EBRT) integrated with conformal high-dose-rate (HDR) brachytherapy boosts. This interim report discusses treatment outcome and prognostic factors using this treatment approach. Methods and Materials: From November 1991 through February 1998, 142 patients with unfavorable prostate cancer were prospectively treated in a dose-escalating trial with pelvic EBRT in combination with outpatient HDR brachytherapy at William Beaumont Hospital. Patients with any of the following characteristics were eligible: pretreatment prostate-specific antigen (PSA) ≥ 10.0 ng/ml, Gleason score ≥ 7, or clinical stage T2b or higher. All patients received pelvic EBRT to a median total dose of 46.0 Gy. Pelvic EBRT was integrated with ultrasound-guided transperineal conformal interstitial iridium-192 HDR implants. From 1991 to 1995, 58 patients underwent three conformal interstitial HDR implants during the first, second, and third weeks of pelvic EBRT. After October 1995, 84 patients received two interstitial implants during the first and third weeks of pelvic EBRT. The dose delivered via interstitial brachytherapy was escalated from 5.50 Gy to 6.50 Gy for each implant in those patients receiving three implants, and subsequently, from 8.25 Gy to 9.50 Gy per fraction in those patients receiving two implants. To improve implant quality and reduce operator dependency, an on-line, image-guided interactive dose optimization program was utilized during each HDR implant. No patient received hormonal therapy unless treatment failure was documented. The median follow-up was 2.1 years (range: 0.2-7.2 years). Biochemical failure was defined according to the American Society for Therapeutic Radiology and Oncology Consensus Panel definition. Results: The pretreatment PSA level was ≥ 10.0 ng/ml in 51% of patients. The

Research on the separation properties of empty-column gas chromatography (EC-GC) and conditions for simulated distillation (SIMDIS).

Science.gov (United States)

Boczkaj, Grzegorz; Kamiński, Marian

2013-10-01

Previous studies have revealed it is possible to separate a high-boiling mixture by gas chromatography in empty fused-silica capillary tubing rather than in columns coated with stationary phase. Chromatographic separation occurs solely on the basis of the different boiling points of the substances separated. The high similarity of such separations to those in classic distillation seems advantageous when gas chromatography is used for simulated distillation. This paper presents results from further research on the separation properties of empty fused silica tubing. The efficiency of this chromatographic system has been examined. The usefulness of such conditions has been studied for simulated distillation, i.e. to determine the boiling-point distribution of complex mixtures, mainly petroleum fractions and products, on the basis of their retention relative to reference substances. The results obtained by use of empty-column gas chromatography (EC-GC) and by use of classical simulated distillation columns have been compared for solutes of different polarity. Studies revealed boiling points determined by EC-GC were more accurate than those obtained by the standard method of simulated distillation.

Study and ICH validation of a reverse-phase liquid chromatographic method for the quantification of the intact monoclonal antibody cetuximab

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Antonio Martínez-Ortega

2016-04-01

Full Text Available Cetuximab (CTX is a potent chimeric mouse/human monoclonal antibody (mAb approved worldwide for treatment of metastatic colorectal cancer. Among the various biological and physical analyses performed for full study on this biopharmaceutic, the determination of the concentration preparations throughout manufacturing and subsequent handling in hospital is particularly relevant. In the present work, the study and validation of a method for quantifying intact CTX by reverse-phase high-performance liquid chromatography with diode array detection ((RPHPLC/DAD is presented. With that end, we checked the performance of a chromatographic method for quantifying CTX and conducted a study to validate the method as stability-indicating in accordance with the International Conference on Harmonization guidelines (ICH for biotechnological drugs; therefore, we evaluated linearity, accuracy, precision, detection and quantification limits, robustness and system suitability. The specificity of the method and the robustness of the mAb formulation against external stress factors were estimated by comprehensive chromatographic analysis by subjecting CTX to several informative stress conditions. As demonstrated, the method is rapid, accurate, and reproducible for CTX quantification. It was also successfully used to quantify CTX in a long-term stability study performed under hospital conditions.

A liquid chromatographic method for determination of theophylline in serum and capillary blood--a comparison.

Science.gov (United States)

Gartzke, J; Jäger, H; Vins, I

1991-01-01

A simple, fast and reliable liquid chromatographic method for the determination of theophylline in serum and capillary blood after a solid phase extraction is described for therapeutic drug monitoring. The employment of capillary blood permits the determination of an individual drug profile and other pharmacokinetic studies in neonates and infants. There were no differences in venous- and capillary-blood levels but these values compared poorly with those in serum. An adjustment of the results by correction of the different volumes of serum and blood by haematocrit was unsuccessful. Differences in the binding of theophylline to erythrocytes could be an explanation for the differences in serum at blood levels of theophylline.

Stochastic resonance is applied to quantitative analysis for weak chromatographic signal of glyburide in plasma

International Nuclear Information System (INIS)

Zhang Wei; Xiang Bingren; Wu Yanwei; Shang Erxin

2005-01-01

Based on the theory of stochastic resonance, a new method carried on the quantitive analysis to weak chromatographic signal of glyburide in plasma, which was embedded in the noise background and the signal-to-noise ratio (SNR) of HPLC-UV is enhanced remarkably. This method enhances the quantification limit to 1 ng ml -1 , which is the same as HPLC-MS, and makes it possible to detect the weak signal accurately by HPLC-UV, which was not suitable before. The results showed good recovery and linear range from 1 to 50 ng ml -1 of glyburide in plasma and the method can be used for quantitative analysis of glyburide

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.

Private Property Rights and Compulsory Acquisition Process in Nigeria: the Past, Present and Future

Directory of Open Access Journals (Sweden)

Akintunde OTUBU

2012-11-01

Full Text Available Objectives: A property right is the exclusive authority to determine how a resource is used, whether that resource is owned by government or by individuals. In the context of land, it is the authority of the land owner to determine its use or otherwise. On the other hand, compulsory acquisition is the process by which government obtain land from private owners for development purposes in the best interest of the community. These diametrically opposed concepts of property rights and compulsory acquisition is reconciled with the payment of compensation for the extinguishment of private property rights. Implications: In Nigeria, these two concepts have a history of mutual conflicts, resulting in congruous resolutions most of the time, until the introduction of the Land Use Act 1978. With the coming of the Act, the pendulum has tilted in favors of compulsory acquisition to the detriment of private property rights; as compensation fails to assuage the loss occasioned by expropriation. Value: The paper explored the dichotomy between private property rights and compulsory acquisition in Nigeria in the last 50 years and submitted that the process under the Land Use Act changed the equilibrium that existed between these two concepts and produced a skewed and unfavorable result to the detriment of private property rights and National economy. It finally proposed a new equitable arrangement to the quagmire.

Chromatographic resolution of closely related species in pharmaceutical chemistry: dehalogenation impurities and mixtures of halogen isomers.

Science.gov (United States)

Regalado, Erik L; Zhuang, Ping; Chen, Yadan; Makarov, Alexey A; Schafer, Wes A; McGachy, Neil; Welch, Christopher J

2014-01-07

In recent years, the use of halogen-containing molecules has proliferated in the pharmaceutical industry, where the incorporation of halogens, especially fluorine, has become vitally important for blocking metabolism and enhancing the biological activity of pharmaceuticals. The chromatographic separation of halogen-containing pharmaceuticals from associated isomers or dehalogenation impurities can sometimes be quite difficult. In an attempt to identify the best current tools available for addressing this important problem, a survey of the suitability of four chromatographic method development platforms (ultra high-performance liquid chromatography (UHPLC), core shell HPLC, achiral supercritical fluid chromatography (SFC) and chiral SFC) for separating closely related mixtures of halogen-containing pharmaceuticals and their dehalogenated isosteres is described. Of the 132 column and mobile phase combinations examined for each mixture, a small subset of conditions were found to afford the best overall performance, with a single UHPLC method (2.1 × 50 mm, 1.9 μm Hypersil Gold PFP, acetonitrile/methanol based aqueous eluents containing either phosphoric or perchloric acid with 150 mM sodium perchlorate) affording excellent separation for all samples. Similarly, a survey of several families of closely related halogen-containing small molecules representing the diversity of impurities that can sometimes be found in purchased starting materials for synthesis revealed chiral SFC (Chiralcel OJ-3 and Chiralpak IB, isopropanol or ethanol with 25 mM isobutylamine/carbon dioxide) as well as the UHPLC (2.1 × 50 mm, 1.8 μm ZORBAX RRHD Eclipse Plus C18 and the Gold PFP, acetonitrile/methanol based aqueous eluents containing phosphoric acid) as preferred methods.

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.

Mass spectrometric protein characterization in proteome analysis using GELoader tip micro-columns packed with various chromatographic material

International Nuclear Information System (INIS)

Larsen, M.R.

2001-01-01

In the early 90'ies mass spectrometry (MS) was introduced as a tool for identifying proteins in protein sequence databases. Since then it has become an integrated tool in protein characterization and is today routinely used to identify proteins separated by gel electrophoresis. A two-tiered mass spectrometric protein identification strategy has recently been proposed. In the first strategy peptide mass maps obtained from the protein of interest are compared with theoretically derived peptide mass maps from proteins in protein sequence databases. If the protein cannot be identified by this strategy, tandem mass spectrometric sequencing is used to generate enough sequence data to identify the protein in protein sequence databases or expressed sequence tag (EST) databases. However, the above strategies primarily identify a protein relatively to the DNA sequence, in which no information about e.g. post-translational modifications (PTMs) is stored. PTMs are known to modify the function, location, solubility and activity of proteins in the cell, and they are therefore very important for understanding living cells. More than 200 different PTMs are known, of which glycosylation, phosphorylation and proteolytic processing are the most common ones. Mass spectrometric analysis of PTMs on gel-separated proteins requires a higher amount of protein than for identification only. In addition, higher sequence coverage from the peptide mass maps or pre-purification of the modified peptides prior to MS analysis, is necessary for detection of putative modified peptides. In this study a multi-tiered strategy, in which GELoader tip micro-columns packed with increasingly more hydrophobic chromatographic material are used in combination with mass spectrometry, is described. The ultimate aim was to gain increased sequence coverage from peptide mixtures derived from gel-separated proteins, in order to locate modified peptides. Graphite powder is described as an alternative to traditional

Chromatographic study of nucleosides and nucleotides of central nervous system. Identification and first results on changes after total gamma irradiation of brain

International Nuclear Information System (INIS)

Valle, C.; Marquer, C.; Pasquier, C.

Changes of brain energetic state and of different levels after irradiation are studied. The results will be compared with the variations of brain electric activity due to irradiation. Using an ion exchange chromatographic method for separation and quantitative analysis of nucleotides, evaluation of adenylic nucleotides in brain rat have been chosen [fr

In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

Energy Technology Data Exchange (ETDEWEB)

Varanusupakul, Pakorn [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)], E-mail: pakorn.v@chula.ac.th; Vora-adisak, Narongchai; Pulpoka, Bancha [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)

2007-08-15

An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na{sub 2}SO{sub 4}. The linear calibration curves were observed for the concentrations ranging from 1 to 300 {mu}g L{sup -1} with the correlation coefficients (R{sup 2}) being greater than 0.99. The method detection limits of most analytes were below 1 {mu}g L{sup -1} except DCAA and MCAA that were 2 and 18 {mu}g L{sup -1}, respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

International Nuclear Information System (INIS)

Varanusupakul, Pakorn; Vora-adisak, Narongchai; Pulpoka, Bancha

2007-01-01

An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na 2 SO 4 . The linear calibration curves were observed for the concentrations ranging from 1 to 300 μg L -1 with the correlation coefficients (R 2 ) being greater than 0.99. The method detection limits of most analytes were below 1 μg L -1 except DCAA and MCAA that were 2 and 18 μg L -1 , respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water

Relevance of the Mention of Antioxidant Properties in Yogurt Labels: In Vitro Evaluation and Chromatographic Analysis

OpenAIRE

Pereira, Eliana; Barros, Lillian; Ferreira, Isabel C. F. R.

2013-01-01

The purpose of the inclusion of fruit (natural additives) in yogurt aims to increase its antioxidant activity and functionality. Herein, a comparative study of the antioxidant potential of yogurts with pieces of various fruits was performed, including yogurts with mention of antioxidant properties in the label. Free radicals scavenging activity, reducing power and inhibition of lipid peroxidation were evaluated by in vitro assays, as were the contents in antioxidants such as phenolics, flavon...

Heterogeneous Ice Nucleation: Interplay of Surface Properties and Their Impact on Water Orientations.

Science.gov (United States)

Glatz, Brittany; Sarupria, Sapna

2018-01-23

Ice is ubiquitous in nature, and heterogeneous ice nucleation is the most common pathway of ice formation. How surface properties affect the propensity to observe ice nucleation on that surface remains an open question. We present results of molecular dynamics studies of heterogeneous ice nucleation on model surfaces. The models surfaces considered emulate the chemistry of kaolinite, an abundant component of mineral dust. We investigate the interplay of surface lattice and hydrogen bonding properties in affecting ice nucleation. We find that lattice matching and hydrogen bonding are necessary but not sufficient conditions for observing ice nucleation at these surfaces. We correlate this behavior to the orientations sampled by the metastable supercooled water in contact with the surfaces. We find that ice is observed in cases where water molecules not only sample orientations favorable for bilayer formation but also do not sample unfavorable orientations. This distribution depends on both surface-water and water-water interactions and can change with subtle modifications to the surface properties. Our results provide insights into the diverse behavior of ice nucleation observed at different surfaces and highlight the complexity in elucidating heterogeneous ice nucleation.

Gas chromatographic-mass spectrometric analysis of biomarkers related to folate and cobalamin status in human serum after dimercaptopropanesulfonate reduction and heptafluorobutyl chloroformate derivatization

Czech Academy of Sciences Publication Activity Database

Šimek, Petr; Hušek, Petr; Zahradníčková, Helena

2008-01-01

Roč. 80, č. 15 (2008), s. 5776-5782 ISSN 0003-2700 R&D Projects: GA ČR GA303/06/1674 Institutional research plan: CEZ:AV0Z50070508 Keywords : biomarkers * gas chromatographic * chloroformate derivatization Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.712, year: 2008

Quantitative HPLC-ICP-MS analysis of antimony redox speciation in complex sample matrices: new insights into the Sb-chemistry causing poor chromatographic recoveries

DEFF Research Database (Denmark)

Hansen, Claus; Schmidt, Bjørn; Larsen, Erik Huusfeldt

2011-01-01

In solution antimony exists either in the pentavalent or trivalent oxidation state. As Sb(III) is more toxic than Sb(V), it is important to be able to perform a quantitative speciation analysis of Sb’s oxidation state. The most commonly applied chromatographic methods used for this redox speciation...

Time-resolved chromatographic analysis and mechanisms in adsorption and catalysis.

Science.gov (United States)

Roubani-Kalantzopoulou, Fani

2009-03-06

The main object of this review is the study of fundamentals of adsorption and heterogeneous catalysis, a benefit for the understanding of adsorptive and catalytic properties. This work aims to define and record, with the utmost accuracy, the phenomena and the possible reactions. A new methodology for the study of the adsorption is presented, which is a version of the well-known inverse gas chromatography. This reversed-flow inverse gas chromatography (RF-IGC) is technically very simple, and it is combined with a mathematical analysis that gives the possibility for the estimation of various physicochemical parameters related to adsorbent or catalyst characterization, under conditions compatible with the operation of real adsorbents and catalysts. On this base, this methodology has been successfully applied to the study of the impact of air pollutants, volatile organic and/or inorganic, on many solids such as marbles, ceramics, oxide-pigments of works of art, building materials, authentic statues of the Greek Archaeological Museums. Moreover, this methodology proved to be a powerful tool for studying the topography of active sites of heterogeneous surfaces in the nano-scale domain. Thus, some very important local quantities for the surface chemistry have been determined experimentally for many solids including thin films. These physicochemical local quantities (among which adsorption energy and entropy, surface diffusion coefficient, probability density function) have been determined from the experimental pairs of height of extra chromatographic peaks and time by a nonlinear least-squares method, through personal computer programs written in GW BASIC and lately in FORTRAN. Through the time-resolved analysis the surface characterization of the examined materials took place. In addition, the kinetic constants responsible for adsorption/desorption and surface chemical reactions have also been calculated. Thus, important answers have been provided to the following

[Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turz) Baill].

Science.gov (United States)

Zhu, Jingbo; Liu, Baoyue; Shan, Shibo; Ding, Yanl; Kou, Zinong; Xiao, Wei

2015-08-01

In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

A single gas chromatograph for accurate atmospheric mixing ratio measurements of CO2, CH4, N2O, SF6 and CO

NARCIS (Netherlands)

van der Laan, S.; Neubert, R. E. M.; Meijer, H. A. J.; Simpson, W.R.

2009-01-01

We present an adapted gas chromatograph capable of measuring simultaneously and semi-continuously the atmospheric mixing ratios of the greenhouse gases CO2, CH4, N2O and SF6 and the trace gas CO with high precision and long-term stability. The novelty of our design is that all species are measured

First-year survival and growth of three species assemblages planted on reclaimed mine land as affected by three levels of silvicultural intensity

Science.gov (United States)

Chad N. Casselman; Thomas R. Fox; James A. Burger

2006-01-01

Surface mined land in the Appalachian coal-producing region have been found to exhibit growing conditions that are unfavorable for the establishment of productive forests including dense ground covers, compacted soil materials, and unfavorable soil chemical properties. To address these concerns, a 3 x 3 x 3 factor random complete block experiment was used to...

The impact of an unfavorable depression course on network size and loneliness in older people: a longitudinal study in the community.

Science.gov (United States)

Houtjes, Wim; van Meijel, Berno; van de Ven, Peter M; Deeg, Dorly; van Tilburg, Theo; Beekman, Aartjan

2014-10-01

This work aims to gain insight into the long-term impact of depression course on social network size and perceived loneliness in older people living in the community. Within a large representative sample of older people in the community (Longitudinal Aging Study Amsterdam (LASA)), participants with clinically relevant levels of depressive symptoms (scores >16 on the Center for Epidemiological Studies Depression Scale) were followed up over a period of 13 years of the LASA study (five waves). General estimating equations were used to estimate the impact of depression course on network size and loneliness and the interaction with gender and age. An unfavorable course of depression was found to be associated with smaller network sizes and higher levels of loneliness over time, especially in men and older participants. The findings of this study stress the importance of clinical attention to the negative consequences of chronicity in depressed older people. Clinicians should assess possible erosion of the social network over time and be aware of increased feelings of loneliness in this patient group. Copyright © 2014 John Wiley & Sons, Ltd.

The Use of TOC Reconciliation as a Means of Establishing the Degree to Which Chromatographic Screening of Plastic Material Extracts for Organic Extractables Is Complete.

Science.gov (United States)

Jenke, Dennis; Couch, Thomas R; Robinson, Sarah J; Volz, Trent J; Colton, Raymond H

2014-01-01

Extracts of plastic packaging, manufacturing, and delivery systems (or their materials of construction) are analyzed by chromatographic methods to establish the system's extractables profile. The testing strategy consists of multiple orthogonal chromatographic methods, for example, gas and liquid chromatography with multiple detection strategies. Although this orthogonal testing strategy is comprehensive, it is not necessarily complete and members of the extractables profile can elude detection and/or accurate identification/quantification. Because the chromatographic methods rarely indicate that some extractables have been missed, another means of assessing the completeness of the profiling activity must be established. If the extracts are aqueous and contain no organic additives (e.g., pH buffers), then they can be analyzed for their total organic carbon content (TOC). Additionally, the TOC of an extract can be calculated based on the extractables revealed by the screening analyses. The measured and calculated TOC can be reconciled to establish the completeness and accuracy of the extractables profile. If the reconciliation is poor, then the profile is either incomplete or inaccurate and additional testing is needed to establish the complete and accurate profile. Ten test materials and components of systems were extracted and their extracts characterized for organic extractables using typical screening procedures. Measured and calculated TOC was reconciled to establish the completeness of the revealed extractables profile. When the TOC reconciliation was incomplete, the profiling was augmented with additional analytical testing to reveal the missing members of the organic extractables profile. This process is illustrated via two case studies involving aqueous extracts of sterile filters. Plastic materials and systems used to manufacture, contain, store, and deliver pharmaceutical products are extracted and the extracts analyzed to establish the materials' (or

Decreased expression of pyruvate dehydrogenase A1 predicts an unfavorable prognosis in ovarian carcinoma.

Science.gov (United States)

Li, Yaqing; Huang, Ruixia; Li, Xiaoli; Li, Xiaoran; Yu, Dandan; Zhang, Mingzhi; Wen, Jianguo; Goscinski, Mariusz Adam; Trope, Claes G; Nesland, Jahn M; Suo, Zhenhe

2016-01-01

Pyruvate dehydrogenase A1 (PDHA1) serves as a gate-keeper enzyme link between glycolysis and the mitochondrial citric acid cycle. The inhibition of PDHA1 in cancer cells can result in an increased Warburg effect and a more aggressive phenotype in cancer cells. This study was conducted to investigate the expression of PDHA1 in ovarian cancer and the correlation between PDHA1 expression and the prognosis of patients. The PDHA1 protein expression in 3 ovarian cancer cell lines (OVCAR-3, SKOV-3 and ES-2) and 248 surgically removed ovarian carcinoma samples was immunocytochemically examined. Statistical analyses were performed to evaluate the correlations between PDHA1 expression and the clinicopathological characteristics of the patients as well as the predictive value of PDHA1. The results showed the presence of variable expression of PDHA1 in the three ovarian cancer cell lines. Of the 248 ovarian cancer tissue specimens, 45 cases (18.1%) were negative in tumor cells for PDHA1, 162 cases (65.3%) displayed a low expression level, and 41 cases (16.5%) had a relatively high PDHA1 staining. The expression of PDHA1 was associated with the histological subtype ( P =0.004) and FIGO stage ( P =0.002). The median OS time in the PDHA1 negative group, low expression group and high expression group were 0.939 years, 1.443 years and 9.900 years, respectively. The median PFS time in the above three groups were 0.287 years, 0.586 years and 9.900 years, respectively. Furthermore, the high expression of PDHA1 in ovarian carcinoma cells was significantly associated with better OS and PFS by statistical analyses. Multivariate analyses showed that PDHA1 expression was also an independent prognostic factor for higher OS in ovarian cancer patients (HR=0.705, 95% CI 0.541-0.918, P =0.01). Our study indicated that the decreased expression of PDHA1 might be an independent prognostic factor in unfavorable outcomes.

Different Chromatographic Methods for Simultaneous Determination of Mefenamic Acid and Two of Its Toxic Impurities.

Science.gov (United States)

Morcoss, Martha M; Abdelwahab, Nada S; Ali, Nouruddin W; Elsaady, Mohammed T

2017-08-01

Two sensitive, accurate and precise chromatographic methods mentioned as TLC-densitometric method and RP-HPLC-DAD method, were developed and validated for the simultaneous determination of mefenamic acid (MEF) and its two toxic impurities, benzoic acid (BA) and 2,3-dimethylaniline (DMA). In the proposed TLC-densitometric method a developing system consisting of chloroform:acetone:acetic acid:ammonia solution(70:30:2:2, v/v/v/v) was used, TLC aluminum plates 60 F254 was used as a stationary phase and the separated bands were UV-scanned at 225 nm. While the proposed RP-HPLC-DAD method depended on chromatographic separation on C18 column using 0.05 M KH2PO4 buffer: acetonitrile (40:60, v/v) as a mobile phase at constant flow rate of 1 mL/min with UV detection at 225 nm. Linear relationships were obtained in the ranges of 0.3-2, 0.3-2 and 0.3-1.8 μg/band (for TLC-densitometric method) and in the ranges of 7-50, 10-50 and 7-50 μg/mL (for HPLC-DAD method) for MEF, BA and DMA, respectively. Factors affecting the developed methods have been studied and optimized. Moreover ,the proposed methods were successfully applied for determination of the studied drug in its pharmaceutical dosage form. The methods showed no significance difference when compared with the reported method using F-test and Student's-t test. The low of detection and quantization limits of the proposed methods get them suitable for quality control and stability studies of MEF in pharmaceutical formulation. The developed methods have advantages of being more selective and sensitive than the published methods. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Determination of carboxylic acids, carbohydrates and metals in different tomato cultivars by HPLC-ICP-AES in a single chromatographic run

OpenAIRE

Paredes Paredes, Eduardo; Maestre, Salvador E.; Prats Moya, Soledad; Todolí Torró, José Luis

2007-01-01

Póster presentado en European Winter Conference on Plasma Spectrochemistry 2007, 18-23 February 2007, Taormina, Italy The determination of carbohydrates, carboxylic acids and metals is a subject of great interest in the field of food science because their presence and concentration can influence on food quality. Besides the study of the profiles of these compounds can permit the discrimination between different varieties of a product. Unfortunately, the usually employed chromatograph...

Current applications of miniaturized chromatographic and electrophoretic techniques in drug analysis.

Science.gov (United States)

Aturki, Zeineb; Rocco, Anna; Rocchi, Silvia; Fanali, Salvatore

2014-12-01

In the last decade, miniaturized separation techniques have become greatly popular in pharmaceutical analysis. Miniaturized separation methods are increasingly utilized in all processes of drug discovery as well as quality control of pharmaceutical preparation. The great advantages presented by the analytical miniaturized techniques, including high separation efficiency and resolution, rapid analysis and minimal consumption of reagents and samples, make them an attractive alternative to the conventional chromatographic methods for drug analysis. The purpose of this review is to give a general overview of the applicability of capillary electrophoresis (CE), capillary electrochromatography (CEC) and micro/capillary/nano-liquid chromatography (micro-LC/CLC/nano-LC) for the analysis of pharmaceutical formulations, active pharmaceutical ingredients (API), drug impurity testing, chiral drug separation, determination of drugs and metabolites in biological fluids. The results concerning the use of CEC, micro-LC, CLC, and nano-LC in the period 2009-2013, while for CE, those from 2012 up to the review draft are here summarized and some specific examples are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Chromatographic determination of clopidogrel bisulfate; detection and quantification of counterfeit Plavix® tablets

Directory of Open Access Journals (Sweden)

Mona E. ElTantawy

2014-06-01

Full Text Available Counterfeiting of pharmaceutical products is a global problem. Upon using quality-ensuring methods of international pharmacopoeias, additional impurities and the low content of the active pharmaceutical ingredients were detected. In this paper, two chromatographic HPLC and TLC-densitometric methods were proposed as fast and reliable methods for detection and quantitation of counterfeit Plavix® tablets. These tablets were chemically counterfeited by aspirin, its degradate salicylic acid and metronidazole which were separated, besides the active ingredient clopidogrel bisulfate, by the proposed methods. Also, counterfeit was in packaging, strips and tablets’ color and these could be seen by visual inspection compared to original drug. The proposed methods can easily differentiate genuine from counterfeited tablets without need of prior separation. The proposed methods were validated according to ICH guidelines and applied to eleven batches, also were compared statistically with the reported one.

High Performance Liquid Chromatographic Analysis of Almotriptan Malate in Bulk and Tablets

Directory of Open Access Journals (Sweden)

Chandra Bala Sekaran

2013-02-01

Full Text Available Purpose: A simple RP-HPLC method has been developed and validated for the determination of almotriptan malate (ATM in bulk and tablets. Methods: Chromatographic separation of ATM was achieved by using a Thermo Scientific C18 column. A Mobile phase containing a mixture of methanol, water and acetic acid (4:8:0.1 v/v was pumped at the flow rate of 1 mL/min. Detection was performed at 227 nm. According to ICH guidelines, the method was validated. Results: The calibration curve was linear in the concentration range 5–60 μg/mL for the ATM with regression coefficient 0.9999. The method was precise with RSD <1.2%. Excellent recoveries of 99.60 - 100.80% proved the accuracy of the method. The limits of detection and quantification were found to be 0.025 and 0.075 μg/mL, respectively. Conclusion: The method was successfully applied for the quantification of ATM in tablets with acceptable accuracy and precision.

Liquid chromatographic and ultraviolet spectrophotometric determination of bevantolol and hydrochlorothiazide in feeds.

Science.gov (United States)

Spurlock, C H; Schneider, H G

1984-01-01

Separate assay methods have been developed for the 2 components of an 80 + 20 drug blend of bevantolol and hydrochlorothiazide (HCT) in admixtures with animal feed. Drug/diet admixtures are extracted with methanol for reverse phase ion-pair liquid chromatographic (LC) assay of bevantolol, and with acetonitrile for ultraviolet spectrophotometric assay of HCT. Bevantolol, a cardioselective beta blocker, is separated from soluble feed components with an RP-18 column, using methanol-water-acetic acid (60 + 40 + 1) containing 0. 005M octane-sulfonic acid, sodium salt, as ion-pairing reagent. HCT is determined spectrophotometrically in acetonitrile extracts, using a suitable blank extract as reference. Average recovery of HCT from an admixture of 0.5 mg blend/g diet is 94.5% +/- 4.3 RSD and at 2.0 mg/g, 101.5% +/- 3.5 RSD. Bevantolol recovery from the same admixtures is 101.8% +/- 2.7 RSD and 99.0% +/- 3.5 RSD, respectively, using the method as described.

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.)

Studies on the properties of poly(ethylene oxide) R-150 water-swollen hydrogel formed by irradiation

International Nuclear Information System (INIS)

Yang Zhanshan; Zhu Nankang; Yang Shuqin; Qiang Yizhong

2000-01-01

The physical and chemical properties of PEO R-150 water-swollen hydrogel films formed by electron beam irradiation are studied and compared with PEO R-150 hydrogel films. The experimental results show that the irradiation dose and mass fraction of the polymer do not produce a significant effect on the gel fraction, of the PEO R-150 water-swollen hydrogel films (P>0.05). The degrees of swelling of the PEO R-150 water-swollen hydrogel films decrease as the irradiation dose increasing (P 0.05). The results indicate that the saturant crosslinking density, the lowest degree of swelling of the PEO R-150 water-swollen hydrogel films produce and unfavorable effect on their machinery strength

EFFECT OF INTERFACIAL ADHESION ON CRYSTALLIZATION AND MECHANICAL PROPERTIES OF POLY (ETHYLENE TEREPHTHALATE)/GLASS BEAD COMPOSITES

Institute of Scientific and Technical Information of China (English)

OU Yuchun; YU Zhongzhen; ZHU Jin; LI Ge; ZHU Shanguang

1996-01-01

The interfacial adhesion between poly (ethylene terephthalate) (PET) and glass bead was investigated by scanning electron microscope and parallel-plate rheometer. Effect of interfacial adhesion on the crystallization and mechanical properties of PET/glass bead composites was also studied by differential scanning calorimeter and mechanical testers.The results obtained indicate that the glass bead has a heterogeneous nucleation effect on the PET crystallization. Although better interfacial adhesion is advantageous to the increase of the tensile strength of the composite, yet it is unfavorable to the crystallization of PET. It should be pointed out that the crystallization rate of filled PET is always higher than that of pure PET, regardless of the state of interfacial adhesion.

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...

32 CFR 644.329 - Army civil works real property.

Science.gov (United States)

2010-07-01

... hinder or prevent disposition, e.g. remoteness of location, unfavorable topography, and lack of legal..., such as telephone, telegraph, electric transmission, oil, gas, and water lines. (vi) Purchase price of...

Chromatographic and Spectrophotometric Analysis of Phenolic Compounds from Fruits of Libidibia ferrea Martius.

Science.gov (United States)

Ferreira, Magda R A; Fernandes, Mônica T M; da Silva, Wliana A V; Bezerra, Isabelle C F; de Souza, Tatiane P; Pimentel, Maria F; Soares, Luiz A L

2016-05-01

Libidibia ferrea (Mart. ex Tul.) L.P. Queiroz (Fabaceae) is a tree which is native to Brazil, widely known as "Jucá," where its herbal derivatives are used in folk medicine with several therapeutic properties. The constituents, which have already been described in the fruit, are mainly hydrolysable tannins (gallic acid [GA] and ellagic acid [EA]). The aim of this study was to investigate the phenolic variability in the fruit of L. ferrea by ultraviolet/visible (UV/VIS) and chromatographic methods (high-performance liquid chromatography [HPLC]/high-performance thin layer chromatography [HPTLC]). Several samples were collected from different regions of Brazil and the qualitative (fingerprints by HPTLC and HPLC) and quantitative analysis (UV/VIS and HPLC) of polyphenols were performed. The HPTLC and HPLC profiles allowed separation and identification of both major analytical markers: EA and GA. The chemical profiles were similar in a number of spots or peaks for the samples, but some differences could be observed in the intensity or area of the analytical markers for HPTLC or HPLC, respectively. Regarding the quantitative analysis, the polyphenolic content by UV/VIS ranged from 13.99 to 37.86 g% expressed as GA or from 10.75 to 29.09 g% expressed as EA. The contents of EA and GA by liquid chromatography-reversed phase (LC-RP) method ranged from 0.57 to 2.68 g% and from 0.54 to 3.23 g%, respectively. The chemical profiles obtained by HPTLC or HPLC, as well as the quantitative analysis by spectrophotometry or LC-RP method, were suitable for discrimination of each herbal sample and can be used as tools for the comparative analysis of the fruits from L. ferrea. The polyphenols of fruits of Libidibia ferrea can be quantified by UV/VIS and HPLCThe HPLC method was able to detect the gallic and ellagic acids in several samples of fruits of Libidibia ferreaThe phenolic profiles of fruits from Libidibia ferrea by HPTLC and HPLC were reproductible. Abbreviations used: HPTLC

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

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.

Prognosis parameters and polarimetric properties of erythrocytes of the patients suffering from arterial hypertension and coronary heart disease at various patterns of left ventricular remodeling

Science.gov (United States)

Ivaschuk, Oleg I.; Kolomoiets, M. Y.; Mikhaliev, K. O.; Chursina, T. Ya.

2011-09-01

The results of examination of 35 arterial hypertension and coronary heart disease patients are presented. The clinical, paraclinical and echocardiographic examinations were performed, and the parameters of prognosis (survival) according to Seattle Heart Failure Model, as well as the optical (polarimetric) properties of erythrocytic suspension were determined. The group of patients under examination was stratified by patterns of remodeling of left ventricle (LV). It was determined that increasing of anisotropy of erythrocytic suspension along LV remodeling patterns continuum correlates with aggravation of structural and functional state of LV and is associated with unfavorable prognosis.

CD117 expression in fibroblasts-like stromal cells indicates unfavorable clinical outcomes in ovarian carcinoma patients.

Directory of Open Access Journals (Sweden)

Ruixia Huang

Full Text Available The stem cell factor (SCF receptor CD117 (c-kit, is widely used for identification of hematopoietic stem cells and cancer stem cells. Moreover, CD117 expression in carcinoma cells indicates a poor prognosis in a variety of cancers. However the potential expression in tumor microenvironment and the biological and clinical impact are currently not reported. The expression of CD117 was immunohistochemically evaluated in a serial of 242 epithelial ovarian cancer (EOC cases. Thirty-eight out of 242 cases were CD117 positive in fibroblast-like stromal cells and 22 cases were positive in EOC cells. Four cases were both positive in fibroblast-like stromal cells and EOC cells for CD117. CD117 expression in fibroblast-like stromal cells in ovarian carcinoma was closely linked to advanced FIGO stage, poor differentiation grade and histological subtype (p<0.05, and it was significantly associated with poor overall survival (OS and progression free survival (PFS (Kaplan-Meier analysis; p<0.05, log-rank test. CD117 expression in ovarian carcinoma cells was not associated with these clinicopathological variables. The CD117 positive fibroblast-like stromal cells were all positive for mesenchymal stem/stromal cell (MSC marker CD73 but negative for fibroblast markers fibroblast activation protein (FAP and α smooth muscle actin (α-SMA, indicating that the CD117+/CD73+ fibroblast-like stromal cells are a subtype of mesenchymal stem cells in tumor stroma, although further characterization of these cells are needed. It is concluded herewith that the presence of CD117+/CD73+ fibroblast-like stromal cells in ovarian carcinoma is an unfavorable clinical outcome indication.

Comparison of two validated gas-chromatographic methods for the determination of trihalomethanes in drinking water Comparação de dois métodos cromatográficos validados para a dosagem de trialometanos em água potável

OpenAIRE

Maria Yumiko Tominaga; Antonio Flavio Mídio

2003-01-01

In this paper the results obtained using two validated gas-chromatographic procedures on drinking water for the determination of trihalomethanes are compared. The volatile compounds, chloroform (CF), bromodichloromethane (BDCM), dibromochloromethane (DBCM) and bromoform (BF) were detected by purge and trap capillary column gas-chromatography with electrolytic conductivity detector ( ELCD) and the simple and rapid gas-chromatographic method by electron capture detector (ECD) after liquid-liqui...

Mixture-mixture design for the fingerprint optimization of chromatographic mobile phases and extraction solutions for Camellia sinensis.

Science.gov (United States)

Borges, Cleber N; Bruns, Roy E; Almeida, Aline A; Scarminio, Ieda S

2007-07-09

A composite simplex centroid-simplex centroid mixture design is proposed for simultaneously optimizing two mixture systems. The complementary model is formed by multiplying special cubic models for the two systems. The design was applied to the simultaneous optimization of both mobile phase chromatographic mixtures and extraction mixtures for the Camellia sinensis Chinese tea plant. The extraction mixtures investigated contained varying proportions of ethyl acetate, ethanol and dichloromethane while the mobile phase was made up of varying proportions of methanol, acetonitrile and a methanol-acetonitrile-water (MAW) 15%:15%:70% mixture. The experiments were block randomized corresponding to a split-plot error structure to minimize laboratory work and reduce environmental impact. Coefficients of an initial saturated model were obtained using Scheffe-type equations. A cumulative probability graph was used to determine an approximate reduced model. The split-plot error structure was then introduced into the reduced model by applying generalized least square equations with variance components calculated using the restricted maximum likelihood approach. A model was developed to calculate the number of peaks observed with the chromatographic detector at 210 nm. A 20-term model contained essentially all the statistical information of the initial model and had a root mean square calibration error of 1.38. The model was used to predict the number of peaks eluted in chromatograms obtained from extraction solutions that correspond to axial points of the simplex centroid design. The significant model coefficients are interpreted in terms of interacting linear, quadratic and cubic effects of the mobile phase and extraction solution components.

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

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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.

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.

Electrochemical reduction of phthalide at carbon cathodes in dimethylformamide: Effects of supporting electrolyte and gas chromatographic injector-port chemistry on the product distribution

International Nuclear Information System (INIS)

Pasciak, Erick M.; Hochstetler, Spencer E.; Mubarak, Mohammad S.; Evans, Dennis H.; Peters, Dennis G.

2013-01-01

Highlights: • Reduction of phthalide gives a radical-anion that undergoes ring-opening in 3.5 s. • Phthalide reduction gives 2-methylbenzoate esters with electrolyte-derived moieties. • Electrolysis of phthalide affords products that depend on the method of analysis. • Upon reduction, phthalide undergoes deuteration in the presence of deuterium oxide. -- Abstract: Cyclic voltammetry and controlled-potential (bulk) electrolysis have been used to investigate the direct reduction of phthalide at carbon electrodes in dimethylformamide (DMF) containing 0.10 M tetramethylammonium perchlorate (TMAP) or tetra-n-butylammonium perchlorate (TBAP). Cyclic voltammograms recorded with a glassy carbon electrode exhibit a single cathodic peak and a corresponding anodic peak that arise, respectively, from one-electron reduction of phthalide to generate a radical-anion intermediate and from reoxidation of the intermediate. At a scan rate of 100 mV s −1 , quasi-reversible behavior is observed (due to ring-opening of the radical-anion), whereas fully reversible behavior is seen at 5 V s −1 or higher. Digital simulation of cyclic voltammograms indicates that the lifetime of the radical-anion is 3.5 s. Bulk electrolysis of phthalide at a reticulated vitreous carbon cathode affords products that depend on the procedure used to analyze the catholyte. Direct injection of catholyte into a gas chromatograph shows phthalide and a 2-methylbenzoate ester bearing an alkyl moiety from the supporting-electrolyte cation. However, if the catholyte is partitioned between diethyl ether and aqueous hydrochloric acid before gas chromatographic analysis, phthalide and 2-methylbenzoic acid are observed. Thermally induced reactions that occur in the injector port of the gas chromatograph are responsible for the formation of the 2-methylbenzoate ester as well as for the phthalide found in all electrolyzed solutions

SIMULTANEOUS ANALYSIS OF AZIDOTHYMIDINE AND ITS MONOPHOSPHATE, DIPHOSPHATE AND TRIPHOSPHATE DERIVATIVES IN BIOLOGICAL-FLUIDS, TISSUE AND CULTURED-CELLS BY A RAPID HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC METHOD

NARCIS (Netherlands)

MOLEMA, G; JANSEN, RW; Visser, Jan; MEIJER, DKF

1992-01-01

A rapid high-performance liquid chromatographic (HPLC) method for the simultaneous analysis of the antiviral drug azidothymidine (AZT), AZT monophosphate, AZT diphosphate and AZT triphosphate, with ultraviolet detection in the nanomolar range, is described. Determination of these compounds in vitro

Studies of post-elution concentration of 99m-Tc eluted from a gel type chromatographic generator

International Nuclear Information System (INIS)

Suzuki, Katia N.; Osso Junior, Joao Alberto

2007-01-01

The radiopharmaceuticals most used in Diagnostic Nuclear Medicine are those labeled with the metastable technetium ( 99m Tc) due to its ideal physical properties of decay (t 1/2 6.01 h, Eγ 140 keV), low cost and availability facilitated through the commercial generator 99 Mo / 99m Tc. This radionuclide is formed by the β - decay of 99 Mo adsorbed on an alumina column of the generator and collected in the form of sodium pertechnetate (Na 99m TcO 4 ) by elution with saline solution (0.9%). The Radiopharmacy Center (CR) of the IPEN-CNEN/SP developed a gel type chromatographic generator of MoZr with 99 Mo produced by 98 Mo(n, γ) 99 Mo reaction that occurs in IEA-R1 Nuclear Reactor. The gel is composed of zirconium molybdate with elution volume of 12 ml with an activity of 11100 MBq (300 mCi) producing a radioactive concentration of 925 MBq (34 mCi) / ml. The fission generator gives a higher radioactive concentration around 1850 MBq (69 mCi) / ml. The aim of this work is to study a system of post-elution concentration using ion exchange cartridges in tandem (cation - anion) for the attainment of a high enough radioactive concentration to meet the demand of market, with a proved quality. This system of concentration will be made based in the technique of solid phase extraction (SPE) using commercial cartridges of extraction, which contains the solid phase and eluent saline solution (0.9%). As the eluent results of this system used in the gel generator of MoZr will be compared with the fission generator currently produced by IPEN-CNEN/SP. (author)

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