[Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography- reversed-phase liquid chromatography].

Science.gov (United States)

Jia, Youmei; Cai, Jianfeng; Xin, Huaxia; Feng, Jiatao; Fu, Yanhui; Fu, Qing; Jin, Yu

2017-06-08

A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography (Pre-2D-HILIC/RPLC) method was established to separate and purify the components in Trachelospermum jasminoides . The pigments and strongly polar components were removed from the crude extract after the active carbon decolorization and solid phase extraction processes. A Click XIon column (250 mm×20 mm, 10 μm) was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC. Finally, 15 fractions were collected under UV-triggered mode. In the second dimensional RPLC, a C18 column (250 mm×20 mm, 5 μm) was selected and water-acetonitrile was used as mobile phases. As a result, 14 compounds with high purity were obtained, which were further identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). Finally, 11 lignan compounds and three flavonoid compounds were obtained. The method has a good orthogonality, and can improve the resolution and the peak capacity. It is significant for the separation of complex components from Trachelospermum jasminoides .

Mobile phase effects on the retention on polar columns with special attention to the dual hydrophilic interaction-reversed-phase liquid chromatography mechanism, a review.

Science.gov (United States)

Jandera, Pavel; Hájek, Tomáš

2018-01-01

Hydrophilic interaction liquid chromatography on polar columns in aqueous-organic mobile phases has become increasingly popular for the separation of many biologically important compounds in chemical, environmental, food, toxicological, and other samples. In spite of many new applications appearing in literature, the retention mechanism is still controversial. This review addresses recent progress in understanding of the retention models in hydrophilic interaction liquid chromatography. The main attention is focused on the role of water, both adsorbed by the column and contained in the bulk mobile phase. Further, the theoretical retention models in the isocratic and gradient elution modes are discussed. The dual hydrophilic interaction liquid chromatography reversed-phase retention mechanism on polar columns is treated in detail, especially with respect to the practical use in one- and two-dimensional liquid chromatography separations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance liquid chromatography using reversed-phase stationary phases dynamically modified with organophosphorus compound for the separation and determination of lanthanoid elements

International Nuclear Information System (INIS)

Tsuyoshi, Akira; Akiba, Kenichi

2000-01-01

An acidic organophosphorus compound, 2-ethylhexylphosphonic acid mono-2-ethlhexyl ester (EHPA), has been applied to reversed-phase high-performance liquid chromatography (RP-HPLC). The reversed-phase stationary phase was dynamically modified with EHPA by flowing the mobile phase of an acetone-water mixture containing the extracting regent. The retention of lanthanoid elements was widely varied by changing the conditions of the mobile phase, i.e., the pH, the EHPA concentration and the acetone content. The selectivity of EHPA is well reflected to the chromatographic systems, and a precise separation of lanthanoid elements was achieved with sufficient resolution. The determination of Sm was examined in the presence of a large amount of Nd. A linear calibration graph was obtained for Sm at the level of 10 -7 mol dm -3 , in the presence of 1x10 -4 mol dm -3 of Nd. (author)

[Determination of glycyrrhizinic acid in biotransformation system by reversed-phase high performance liquid chromatography].

Science.gov (United States)

Li, Hui; Lu, Dingqiang; Liu, Weimin

2004-05-01

A method for determining glycyrrhizinic acid in the biotransformation system by reversed-phase high performance liquid chromatography (RP-HPLC) was developed. The HPLC conditions were as follows: Hypersil C18 column (4.6 mm i.d. x 250 mm, 5 microm) with a mixture of methanol-water-acetic acid (70:30:1, v/v) as the mobile phase; flow rate at 1.0 mL/min; and UV detection at 254 nm. The linear range of glycyrrhizinic acid was 0.2-20 microg. The recoveries were 98%-103% with relative standard deviations between 0.16% and 1.58% (n = 3). The method is simple, rapid and accurate for determining glycyrrhizinic acid.

Preparation and characterization of a new microwave immobilized poly(2-phenylpropyl)methylsiloxane stationary phase for reversed phase high-performance liquid chromatography.

Science.gov (United States)

Begnini, Fernanda R; Jardim, Isabel C S F

2013-07-05

A new reversed phase high-performance liquid chromatography (RP-HPLC) stationary phase was prepared and its chromatographic and physical-chemical properties were evaluated. The new stationary phase was prepared with a silica support and poly(2-phenylpropyl)methylsiloxane (PPPMS), a phenyl type polysiloxane copolymer. Since this is a new copolymer and there is little information in the literature, it was submitted to physical-chemical characterization by infrared spectroscopy and thermogravimetry. The chromatographic phase was prepared through sorption and microwave immobilization of the copolymer onto a silica support. The chromatographic performance was evaluated by employing test procedures suggested by Engelhardt and Jungheim, Tanaka and co-workers, Neue, and Szabó and Csató. These test mixtures provide information about the hydrophobic selectivity, silanophilic activity, ion-exchange capacity, shape selectivity and interaction with polar analytes of the new Si-PPPMS reversed phase. Stability tests were developed using accelerated aging tests under both basic and acidic conditions to provide information about the lifetime of the packed columns. Copyright © 2013 Elsevier B.V. All rights reserved.

Analysis of proinsulin and its conversion products by reversed-phase high-performance liquid chromatography

DEFF Research Database (Denmark)

Linde, S; Welinder, B S; Nielsen, Jens Høiriis

1993-01-01

. Most mammals produce a single insulin, but in rodents two non-allelic insulin genes are expressed. There is an inverse ratio between the two insulins in rats and mice, the reason for this being unknown. It has been suggested that differences in transcription, translation (biosynthesis) and...... PIM (intact proinsulin or its intermediates) has been incompletely determined. Studies of the biosynthesis of proinsulins and their conversion with the purpose of revealing some of these points depend on accessible reversed-phase high-performance liquid chromatographic (RP-HPLC) analyses capable...

Liquid-liquid and liquid-solid phase separation and flocculation for a charged colloidal dispersion

International Nuclear Information System (INIS)

Lai, S.K.; Wu, K.L.

2002-01-01

We model the intercolloidal interaction by a hard-sphere Yukawa repulsion to which is added the long-range van der Waals attraction. In comparison with the Derjaguin-Landau-Verwey-Overbeek repulsion, the Yukawa repulsion explicitly incorporates the spatial correlations between colloids and small ions. As a result, the repulsive part can be expressed analytically and has a coupling strength depending on the colloidal volume fraction. By use of this two-body potential of mean force and in conjunction with a second-order thermodynamic perturbation theory, we construct the colloidal Helmholtz free energy and use it to calculate the thermodynamic quantities, pressure and chemical potential, needed in the determination of the liquid-liquid and liquid-solid phase diagrams. We examine, in an aqueous charged colloidal dispersion, the effects of the Hamaker constant and particle size on the conformation of a stable liquid-liquid phase transition calculated with respect to the liquid-solid coexistence phases. We find that there exists a threshold Hamaker constant or particle size whose value demarcates the stable liquid-liquid coexistence phases from their metastable counterparts. Applying the same technique and using the energetic criterion, we extend our calculations to study the flocculation phenomenon in aqueous charged colloids. Here, we pay due attention to determining the loci of a stability curve stipulated for a given temperature T 0 , and obtain the parametric phase diagram of the Hamaker constant vs the coupling strength or, at given surface potential, the particle size. By imposing T 0 to be the critical temperature T c , i.e., setting k B T 0 (=k B T c ) equal to a reasonable potential barrier, we arrive at the stability curve that marks the irreversible reversible phase transition. The interesting result is that there occurs a minimum size for the colloidal particles below (above) which the colloidal dispersion is driven to an irreversible (reversible) phase

[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.

Characterization of retentivity of reversed phase liquid chromatography columns.

Science.gov (United States)

Ying, P T; Dorsey, J G

1991-03-01

There are dozens of commercially available reversed phase columns, most marketed as C-8 or C-18 materials, but with no useful way of classifying their retentivity. A useful way of ranking these columns in terms of column "strength" or retentivity is presented. The method utilizes a value for ln k'(w), the estimated retention of a solute from a mobile phase of 100% water, and the slope of the plot of ln k' vsE(T)(30), the solvent polarity. The method is validated with 26 solutes varying in ln k'(w) from about 2 to over 20, on 14 different reversed phase columns. In agreement with previous work, it is found that the phase volume ratio of the column is the most important parameter in determining retentivity. It is strongly suggested that manufacturers adopt a uniform method of calculating this value and that it be made available in advertising, rather than the uninterpretable "% carbon".

Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

International Nuclear Information System (INIS)

Kim, Jeong Soo; Kim, Keon; Kim, Do Hwan

2012-01-01

A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL

Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

Energy Technology Data Exchange (ETDEWEB)

Kim, Jeong Soo; Kim, Keon [Korea Univ., Seoul (Korea, Republic of); Kim, Do Hwan [Daegu Univ., Gyeongsan (Korea, Republic of)

2012-12-15

A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

Optimizing gradient conditions in online comprehensive two-dimensional reversed-phase liquid chromatography by use of the linear solvent strength model

DEFF Research Database (Denmark)

Græsbøll, Rune; Janssen, Hans-Gerd; Christensen, Jan H.

2017-01-01

The linear solvent strength model was used to predict coverage in online comprehensive two-dimensional reversed-phase liquid chromatography. The prediction model uses a parallelogram to describe the separation space covered with peaks in a system with limited orthogonality. The corners of the par......The linear solvent strength model was used to predict coverage in online comprehensive two-dimensional reversed-phase liquid chromatography. The prediction model uses a parallelogram to describe the separation space covered with peaks in a system with limited orthogonality. The corners...... of the parallelogram are assumed to behave like chromatographic peaks and the position of these pseudo-compounds was predicted. A mix of 25 polycyclic aromatic compounds were used as a test. The precision of the prediction, span 0-25, was tested by varying input parameters, and was found to be acceptable with root...... factors were low, or when gradient conditions affected parameters not included in the model, e.g. second dimension gradient time affects the second dimension equilibration time. The concept shows promise as a tool for gradient optimization in online comprehensive two-dimensional liquid chromatography...

Leukotriene B4 catabolism: quantitation of leukotriene B4 and its omega-oxidation products by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Shak, S

1987-01-01

LTB4 and its omega-oxidation products may be rapidly, sensitively, and specifically quantitated by the methods of solid-phase extraction and reversed-phase high-performance liquid chromatography (HPLC), which are described in this chapter. Although other techniques, such as radioimmunoassay or gas chromatography-mass spectrometry, may be utilized for quantitative analysis of the lipoxygenase products of arachidonic acid, only the technique of reversed-phase HPLC can quantitate as many as 10 metabolites in a single analysis, without prior derivatization. In this chapter, we also reviewed the chromatographic theory which we utilized in order to optimize reversed-phase HPLC analysis of LTB4 and its omega-oxidation products. With this information and a gradient HPLC system, it is possible for any investigator to develop a powerful assay for the potent inflammatory mediator, LTB4, or for any other lipoxygenase product of arachidonic acid.

Purification of lignans from Fructus Arctii using off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography.

Science.gov (United States)

Yang, Bichao; Xin, Huaxia; Wang, Feier; Cai, Jianfeng; Liu, Yanfang; Fu, Qing; Jin, Yu; Liang, Xinmiao

2017-08-01

As a common traditional Chinese medicine, Fructus Arctii has important clinical medical values. Its main components are lignans, which are difficult to separate and analyze because of the complex composition, similar chemical structures, and close properties. In this study, an off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method, as well as an effective sample pretreatment method based on hydrophilic interaction chromatography material, was developed to enrich the minor lignan fractions and obtain high-purity compounds. In total, 12 high-purity compounds were isolated from Fructus Arctii. Their structures were identified by using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy, which showed that all were lignans and that most of them were isomers. The results demonstrated the effective off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method for the purification of lignans from Fructus Arctii. The separation protocol established here will be beneficial for the separation of complex samples from other kinds of natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polarity-based fractionation in proteomics: hydrophilic interaction vs reversed-phase liquid chromatography.

Science.gov (United States)

Jafari, M; Mirzaie, M; Khodabandeh, M; Rezadoost, H; Ghassempour, A; Aboul-Enein, H Y

2016-07-01

During recent decades, hydrophilic interaction liquid chromatography (HILIC) ahs been introduced to fractionate or purify especially polar solutes such as peptides and proteins while reversed-phase liquid chromatography (RPLC) is also a common strategy. RPLC is also a common dimension in multidimensional chromatography. In this study, the potential of HILIC vs RPLC chromatography was compared for proteome mapping of human peripheral blood mononuclear cell extract. In HILIC a silica-based stationary phase and for RPLC a C18 column were applied. Then separated proteins were eluted to an ion trap mass spectrometry system. Our results showed that the HILIC leads to more proteins being identified in comparison to RPLC. Among the total 181 identified proteins, 56 and 38 proteins were fractionated specifically by HILIC and RPLC, respectively. In order to demonstrate this, the physicochemical properties of identified proteins such as polarity and hydrophobicity were considered. This analysis indicated that polarity may play a major role in the HILIC separation of proteins vs RPLC. Using gene ontology enrichment analysis, it was also observed that differences in physicochemical properties conform to the cellular compartment and biological features. Finally, this study highlighted the potential of HILIC and the great orthogonality of RPLC in gel-free proteomic studies. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Retention prediction and hydrophobicity estimation of weak acidic compounds by reversed-phase liquid chromatography using acetic and perchloric acids as ion suppressors.

Science.gov (United States)

Han, Shu-ying; Ming, Xin; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

2010-11-01

Simple acids are usually applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography. The purpose of this study is to investigate the retention behavior of various weak acidic compounds (monoprotic, diprotic, triprotic, and tetraprotic acids) using acetic or perchloric acid as ion suppressor in a binary hydroorganic mobile phase. The apparent n-octanol-water partition coefficient (K(ow)") was proposed to calibrate the n-octanol-water partition coefficient (K(ow)) of weak acidic compound. LogK(ow)" was found to have a better linear correlation with logk(w), the logarithm of the retention factor obtained by extrapolating to neat aqueous fraction of the mobile phase, for all weakly ionizable acidic compounds. This straightforward relationship offers a potential medium for direct measurement of K(ow) data of weak acidic analytes and can be used to predict retention behavior of these compounds in the ion suppression reversed-phase liquid chromatographic mode.

Separation of deuteriated isotopomers of dopamine by ion-pair reversed-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Masters, C.F.; Markey, S.P.; Mefford, I.N.; Duncan, M.W.

1988-01-01

The ion-pair reversed-phase separation of dopamine and deuterium-substituted dopamine isotopomers is described. Chromatographic parameters and deuterium isotope effects governing the resolution are examined and compared to the factors regulating the resolution are examined and compared to the factors regulating the resolution of the chemically distinct entities dopamine, norepinephrine, and epinephrine. The potential utility of the [ 2 H 7 ]dopamine, isotopomer as an internal standard for the high-performance liquid chromatography analysis of dopamine is demonstrated by using aluminum oxide extraction prior to chromatographic separation

Retention of nucleic acids in ion-pair reversed-phase high-performance liquid chromatography depends not only on base composition but also on base sequence.

Science.gov (United States)

Qiao, Jun-Qin; Liang, Chao; Wei, Lan-Chun; Cao, Zhao-Ming; Lian, Hong-Zhen

2016-12-01

The study on nucleic acid retention in ion-pair reversed-phase high-performance liquid chromatography mainly focuses on size-dependence, however, other factors influencing retention behaviors have not been comprehensively clarified up to date. In this present work, the retention behaviors of oligonucleotides and double-stranded DNAs were investigated on silica-based C 18 stationary phase by ion-pair reversed-phase high-performance liquid chromatography. It is found that the retention of oligonucleotides was influenced by base composition and base sequence as well as size, and oligonucleotides prone to self-dimerization have weaker retention than those not prone to self-dimerization but with the same base composition. However, homo-oligonucleotides are suitable for the size-dependent separation as a special case of oligonucleotides. For double-stranded DNAs, the retention is also influenced by base composition and base sequence, as well as size. This may be attributed to the interaction of exposed bases in major or minor grooves with the hydrophobic alky chains of stationary phase. In addition, no specific influence of guanine and cytosine content was confirmed on retention of double-stranded DNAs. Notably, the space effect resulted from the stereostructure of nucleic acids also influences the retention behavior in ion-pair reversed-phase high-performance liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

Science.gov (United States)

Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

2016-01-01

A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

QUANTITATIVE ION-PAIR EXTRACTION OF 4(5)-METHYLIMIDAZOLE FROM CARAMEL COLOR AND ITS DETERMINATION BY REVERSED-PHASE ION-PAIR LIQUID-CHROMATOGRAPHY

DEFF Research Database (Denmark)

Thomsen, Mohens; Willumsen, Dorthe

1981-01-01

A procedure for quantitative ion-pair extraction of 4(5)-methylimidazole from caramel colour using bis(2-ethylhexyl)phosphoric acid as ion-pairing agent has been developed. Furthermore, a reversed-phase ion-pair liquid chromatographic separation method has been established to analyse the content...

Molecular-level characterization of crude oil compounds combining reversed-phase high-performance liquid chromatography with off-line high-resolution mass spectrometry

Science.gov (United States)

Sim, Arum; Cho, Yunju; Kim, Daae; Witt, Matthias; Birdwell, Justin E.; Kim, Byung Ju; Kim, Sunghwan

2014-01-01

A reversed-phase separation technique was developed in a previous study (Loegel et al., 2012) and successfully applied to the de-asphalted fraction of crude oil. However, to the best of our knowledge, the molecular-level characterization of oil fractions obtained by reversed-phase high-performance liquid chromatography (HPLC) coupled with high-resolution mass spectrometry (MS) has not yet been reported. A detailed characterization of the oil fractions prepared by reversed-phase HPLC was performed in this study. HPLC fractionation was carried out on conventional crude oil and an oil shale pyrolysate. The analyses of the fractions showed that the carbon number of alkyl chains and the double bond equivalent (DBE) value were the major factors determining elution order. The compounds with larger DBE (presumably more condensed aromatic structures) and smaller carbon number (presumably compounds with short side chains) were eluted earlier but those compounds with lower DBE values (presumably less aromatic structures) and higher carbon number (presumably compounds with longer alkyl chains) eluted later in the chromatograms. This separation behavior is in good agreement with that expected from the principles of reversed-phase separation. The data presented in this study show that reversed-phase chromatography is effective in separating crude oil compounds and can be combined with ultrahigh-resolution MS data to better understand natural oils and oil shale pyrolysates.

Simultaneous quantification of porcine myocardial adenine nucleotides and creatine phosphate by ion-pair reverse-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Cordis, G.A.; Das, D.K.

1987-01-01

In order to follow the energy metabolism and the levels of high-energy phosphate compounds in porcine myocardium subjected to ischemic insult, it was necessary to develop a high-performance liquid chromatography (HPLC) method where creatine phosphate (CP) and the adenine nucleotides could be measured simultaneously in a single run. Currently available ion-pair reverse-phase HPLC methods require a separate injection with a change in wavelength and mobile phase in order to measure the creatine phosphate, while baseline separation of AMP is lacking. The ion-exchange HPLC method includes a simultaneous determination, but the baseline drifts due to the gradient and baseline separation of AMP is not achieved. In the following ion-pair reverse-phase HPLC method, simultaneous measurements of porcine myocardial adenine nucleotides and creatine phosphate were achieved along with a stable baseline and homogeneous baseline separation of each measured compound, allowing accurate quantification

Thermodynamic and kinetic characterization of polycyclic aromatic hydrocarbons in reversed-phase liquid chromatography.

Science.gov (United States)

Howerton, Samuel B; McGuffin, Victoria L

2003-07-15

The retention of six polycyclic aromatic hydrocarbons (PAHs) was characterized by reversed-phase liquid chromatography. The PAHs were detected by laser-induced fluorescence at four points along an optically transparent capillary column. The profiles were characterized in space and time using an exponentially modified Gaussian equation. The resulting parameters were used to calculate the retention factors, as well as the concomitant changes in molar enthalpy and molar volume, for each PAH on monomeric (2.7 micromol/m2) and polymeric (5.4 micromol/m2) octadecylsilica. The changes in molar enthalpy become more exothermic as ring number increases and as annelation structure becomes less condensed. The changes in molar volume become more negative as ring number increases for the planar PAHs, but are positive for the nonplanar solutes. In addition, the rate constants, as well as the concomitant activation enthalpy and activation volume, are calculated for the first time. The kinetic data demonstrate that many of the PAHs exhibit very fast transitions between the mobile and stationary phases. The transition state is very high in energy, and the activation enthalpies and volumes become greater as ring number increases and as annelation structure becomes less condensed. The changes in thermodynamic and kinetic behavior are much more pronounced for the polymeric phase than for the monomeric phase.

A new imidazolium-embedded C{sub 18} stationary phase with enhanced performance in reversed-phase liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Qiu Hongdeng [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou 730000 (China); Mallik, Abul K. [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Takafuji, Makoto [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Kumamoto Institute for Photo-Electro Organics (Phoenics), Kumamoto 862-0901 (Japan); Liu Xia; Jiang Shengxiang [Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou 730000 (China); Ihara, Hirotaka, E-mail: ihara@kumamoto-u.ac.jp [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Kumamoto Institute for Photo-Electro Organics (Phoenics), Kumamoto 862-0901 (Japan)

2012-08-13

Highlights: Black-Right-Pointing-Pointer Imidazolium-embedded C{sub 18} stationary phase was prepared and characterized. Black-Right-Pointing-Pointer Enhanced chromatographic selectivity was observed in SiImC{sub 18} column. Black-Right-Pointing-Pointer Seven nucleosides and bases were separated using only water as eluent within 8 min. Black-Right-Pointing-Pointer Multiple-interactions induced by embedded polar imidazolium was investigated. - Abstract: In this paper, a new imidazolium-embedded C{sub 18} stationary phase (SiImC{sub 18}) for reversed-phase high-performance liquid chromatography is described. 1-Allyl-3-octadecylimidazolium bromide ionic liquid compound having a long alkyl chain and reactive groups was newly prepared and grafted onto 3-mercaptopropyltrimethoxysilane-modified silica via a surface-initiated radical-chain transfer addition reaction. The SiImC{sub 18} obtained was characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, diffuse reflectance infrared Fourier transform, and solid-state {sup 13}C and {sup 29}Si cross-polarization/magic angle spinning nuclear magnetic resonance spectroscopy. The selectivity toward polycyclic aromatic hydrocarbons relative to that toward alkylbenzenes exhibited by SiImC{sub 18} was higher than the corresponding selectivity exhibited by a conventional octadecyl silica (ODS) column, which could be explained by electrostatic {pi}-{pi} interaction cationic imidazolium and electron-rich aromatic rings. On the other hand, SiImC{sub 18} also showed high selectivity for polar compounds, which was based on the multiple interaction and retention mechanisms of this phase with different analytes. 1,6-Dinitropyrene and 1,8-dinitropyrene, which form a positional isomer pair of dipolar compounds, were separated successfully with the SiImC{sub 18} phase. Seven nucleosides and bases (i.e. cytidine, uracil, uridine, thymine, guanosine, xanthosine, and adenosine) were separated using only water as

Effect of molecular interactions on retention and selectivity in reversed-phase liquid chromatography.

Science.gov (United States)

Szepesy, László

2002-06-25

The linear solvation energy relationships (LSERs) have been applied in the last years for description and prediction of retention and selectivity in reversed-phase liquid chromatography with good results. Widely different stationary phases have been compared and characterized by LSERs. In recent publications the influence of the type of the organic moderator and the composition of the mobile phase have also been described. However, the influence of the molecular properties of the solutes to be separated has never been discussed. According to the LSER model variation in retention factors (log k) with solute structure can be related to their potential for various intermolecular interactions. The retention factor is given as the sum of the terms of the LSER equation representing various types of molecular interactions. For this reason the influence of the structure and molecular properties of the solutes to be separated can also be investigated using the LSER equation. In this study we shall demonstrate how the specific molecular interactions influence chromatographic retention and selectivity. We intend to show that retention and selectivity depend on all participants of the system. In addition to the structure and properties of the stationary phase and the type and composition of the mobile phase the molecular properties of the solutes, characterized by the solvation parameters, will also influence the type and extent of the various molecular interactions governing retention and selectivity.

Systematic Comparison of Reverse Phase and Hydrophilic Interaction Liquid Chromatography Platforms for the Analysis of N-linked Glycans

Science.gov (United States)

Walker, S. Hunter; Carlisle, Brandon C.; Muddiman, David C.

2013-01-01

Due to the hydrophilic nature of glycans, reverse phase chromatography has not been widely used as a glycomic separation technique coupled to mass spectrometry. Other approaches such as hydrophilic interaction chromatography and porous graphitized carbon chromatography are often employed, though these strategies frequently suffer from decreased chromatographic resolution, long equilibration times, indefinite retention, and column bleed. Herein, it is shown that through an efficient hydrazone formation derivatization of N-linked glycans (∼4 hr of additional sample preparation time which is carried out in parallel), numerous experimental and practical advantages are gained when analyzing the glycans by online reverse phase chromatography. These benefits include an increased number of glycans detected, increased peak capacity of the separation, and the ability to analyze glycans on the identical liquid chromatography-mass spectrometry platform commonly used for proteomic analyses. The data presented show that separation of derivatized N-linked glycans by reverse phase chromatography significantly out-performs traditional separation of native or derivatized glycans by hydrophilic interaction chromatography. Furthermore, the movement to a more ubiquitous separation technique will afford numerous research groups the opportunity to analyze both proteomic and glycomic samples on the same platform with minimal time and physical change between experiments, increasing the efficiency of ‘multi-omic’ biological approaches. PMID:22954204

Online combination of reversed-phase/reversed-phase and porous graphitic carbon liquid chromatography for multicomponent separation of proteomics and glycoproteomics samples.

Science.gov (United States)

Lam, Maggie P Y; Lau, Edward; Siu, S O; Ng, Dominic C M; Kong, Ricky P W; Chiu, Philip C N; Yeung, William S B; Lo, Clive; Chu, Ivan K

2011-11-01

In this paper, we describe an online combination of reversed-phase/reversed-phase (RP-RP) and porous graphitic carbon (PGC) liquid chromatography (LC) for multicomponent analysis of proteomics and glycoproteomics samples. The online RP-RP portion of this system provides comprehensive 2-D peptide separation based on sequence hydrophobicity at pH 2 and 10. Hydrophilic components (e.g. glycans, glycopeptides) that are not retained by RP are automatically diverted downstream to a PGC column for further trapping and separation. Furthermore, the RP-RP/PGC system can provide simultaneous extension of the hydropathy range and peak capacity for analysis. Using an 11-protein mixture, we found that the system could efficiently separate native peptides and released N-glycans from a single sample. We evaluated the applicability of the system to the analysis of complex biological samples using 25 μg of the lysate of a human choriocarcinoma cell line (BeWo), confidently identifying a total of 1449 proteins from a single experiment and up to 1909 distinct proteins from technical triplicates. The PGC fraction increased the sequence coverage through the inclusion of additional hydrophilic sequences that accounted for up to 6.9% of the total identified peptides from the BeWo lysate, with apparent preference for the detection of hydrophilic motifs and proteins. In addition, RP-RP/PGC is applicable to the analysis of complex glycomics samples, as demonstrated by our analysis of a concanavalin A-extracted glycoproteome from human serum; in total, 134 potentially N-glycosylated serum proteins, 151 possible N-glycosylation sites, and more than 40 possible N-glycan structures recognized by concanavalin A were simultaneously detected. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid Quantitative Analysis of Naringenin in the Fruit Bodies of Inonotus vaninii by Two-phase Acid Hydrolysis Followed by Reversed Phase-high Performance Liquid Chromatography-ultra Violet.

Science.gov (United States)

Guohua, Xia; Pan, Ruirong; Bao, Rui; Ge, Yanru; Zhou, Cunshan; Shen, Yuping

2017-01-01

Sanghuang is one of mystical traditional Chinese medicines recorded earliest 2000 years ago, that included various fungi of Inonotus genus and was well-known for antitumor effect in modern medicine. Inonotus vaninii is grown in natural forest of Northeastern China merely and used as Sanghuang commercially, but it has no quality control specification until now. This study was to establish a rapid method of two-phase acid hydrolysis followed by reversed phase-high performance liquid chromatography-ultra violet (RP-HPLC-UV) to quantify naringenin in the fruit body of I. vaninii . Sample solution was prepared by pretreatment of raw material in two-phase acid hydrolysis and the hydrolysis technology was optimized. After reconstitution, analysis was performed using RP-HPLC-UV. The method validation was investigated and the naringenin content of sample and comparison were determined. The naringenin was obtained by two-phase acid hydrolysis method, namely, 10.0 g of raw material was hydrolyzed in 200 mL of 1% sulfuric acid aqueous solution (v/v) and 400 mL of chloroform in oil bath at 110°C for 2 h. Good linearity ( r = 0.9992) was achieved between concentration of analyte and peak area. The relative standard deviation (RSD) of precision was 2.47% and the RSD of naringenin contents for repeatability was 3.13%. The accuracy was supported with recoveries at 96.37%, 97.30%, and 99.31%. The sample solution prepared using the proposed method contained higher content of naringenin than conventional method and was stable for 8 h. Due to the high efficiency of sample preparation and high reliability of the HPLC method, it is feasible to use this method for routine analysis of naringenin in the fungus. A convenient two-phase acid hydrolysis was employed to produce naringenin from raw material, and then an efficient and reliable reversed phase-high performance liquid chromatography-ultra violet method was established to monitor naringenin in the fruit bodies of Inonotus vaninii

Enantiomeric separation of type I and type II pyrethroid insecticides with different chiral stationary phases by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Zhang, Ping; Yu, Qian; He, Xiulong; Qian, Kun; Xiao, Wei; Xu, Zhifeng; Li, Tian; He, Lin

2018-04-01

The enantiomeric separation of type I (bifenthrin, BF) and type II (lambda-cyhalothrin, LCT) pyrethroid insecticides on Lux Cellulose-1, Lux Cellulose-3, and Chiralpak IC chiral columns was investigated by reversed-phase high-performance liquid chromatography. Methanol/water or acetonitrile/water was used as mobile phase at a flow rate of 0.8 mL/min. The effects of chiral stationary phase, mobile phase composition, column temperature, and thermodynamic parameters on enantiomer separation were carefully studied. Bifenthrin got a partial separation on Lux Cellulose-1 column and baseline separation on Lux Cellulose-3 column, while LCT enantiomers could be completely separated on both Lux Cellulose-1 and Lux Cellulose-3 columns. Chiralpak IC provided no separation ability for both BF and LCT. Retention factor (k) and selectivity factor (α) decreased with the column temperature increasing from 10°C to 40°C for both BF and LCT enantiomers. Thermodynamic parameters including ∆H and ∆S were also calculated, and the maximum R s were not always obtained at lowest temperature. Furthermore, the quantitative analysis methods for BF and LCT enantiomers in soil and water were also established. Such results provide a new approach for pyrethroid separation under reversed-phase condition and contribute to environmental risk assessment of pyrethroids at enantiomer level. © 2017 Wiley Periodicals, Inc.

Separation and determination of synthetic impurities of difloxacin by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Rao, R Nageswara; Nagaraju, V

2004-11-19

A simple and rapid reversed-phase high-performance liquid chromatographic method for separation and determination of process-related impurities of difloxacin (DFL) was developed. The separation was achieved on a reversed-phase C(18) column using methanol-water-acetic acid (78:21.9:0.1, v/v/v) as a mobile solvent at a flow rate of 1.0 ml/min at 28 degrees C using UV detection at 230 nm. It was linear over a range of 0.03 x 10(-6) to 1.60 x 10(-6)g for process related impurities and 0.05 x 10(-6) to 2.40 x 10(-6)g for difloxacin. The detection limits were 0.009 x 10(-6) to 0.024 x 10(-6)g for all the compounds examined. The recoveries were found to be in the range of 97.6-102.0% for impurities as well as difloxacin. The precision and robustness of the method were evaluated. It was used for not only quality assurance, but also monitoring the synthetic reactions involved in the process development work of difloxacin. The method was found to be specific, precise and reliable for the determination of unreacted levels of raw materials, intermediates in the reaction mixtures and the finished products of difloxacin.

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

Sequence-dependent separation of trinucleotides by ion-interaction reversed-phase liquid chromatography A structure-retention study assisted by soft-modelling and molecular dynamics

Czech Academy of Sciences Publication Activity Database

Mikulášek, K.; Jaroň, Kamil S.; Kulhánek, P.; Bittová, M.; Havliš, J.

2016-01-01

Roč. 1469, October (2016), s. 88-95 ISSN 0021-9673 Institutional support: RVO:68081766 Keywords : Sequence-dependent separation * Ion-interaction reversed-phase liquid chromatography * Trinucleotides * Oligonucleotide sequence isomers * QSRR * Molecular dynamics Subject RIV: CE - Biochemistry Impact factor: 3.981, year: 2016

Quantitative structure-retention relationships of pesticides in reversed-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Aschi, Massimiliano; D'Archivio, Angelo Antonio; Maggi, Maria Anna; Mazzeo, Pietro; Ruggieri, Fabrizio

2007-01-01

In this paper, a quantitative structure-retention relationships (QSRR) method is employed to predict the retention behaviour of pesticides in reversed-phase high-performance liquid chromatography (HPLC). A six-parameter nonlinear model is developed by means of a feed-forward artificial neural network (ANN) with back-propagation learning rule. Accurate description of the retention factors of 26 compounds including commonly used insecticides, herbicides and fungicides and some metabolites is successfully achieved. In addition to the acetonitrile content, included to describe composition of the water-acetonitrile mobile phase, the octanol-water partition coefficient (from literature) and four quantum chemical descriptors are considered to account for the effect of solute structure on the retention. These are: the total dipole moment, the mean polarizability, the anisotropy of polarizability and a descriptor of hydrogen bonding ability based on the atomic charges on hydrogen bond donor and acceptor chemical functionalities. The proposed nonlinear QSRR model exhibits a high degree of correlation between observed and computed retention factors and a good predictive performance in wide range of mobile phase composition (40-65%, v/v acetonitrile) that supports its application for the prediction of the chromatographic behaviour of unknown pesticides. A multilinear regression model based on the same six descriptors shows a significantly worse predictive capability

Quantitative structure-retention relationships of pesticides in reversed-phase high-performance liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Aschi, Massimiliano [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); D' Archivio, Angelo Antonio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)]. E-mail: darchivi@univaq.it; Maggi, Maria Anna [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); Mazzeo, Pietro [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); Ruggieri, Fabrizio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)

2007-01-23

In this paper, a quantitative structure-retention relationships (QSRR) method is employed to predict the retention behaviour of pesticides in reversed-phase high-performance liquid chromatography (HPLC). A six-parameter nonlinear model is developed by means of a feed-forward artificial neural network (ANN) with back-propagation learning rule. Accurate description of the retention factors of 26 compounds including commonly used insecticides, herbicides and fungicides and some metabolites is successfully achieved. In addition to the acetonitrile content, included to describe composition of the water-acetonitrile mobile phase, the octanol-water partition coefficient (from literature) and four quantum chemical descriptors are considered to account for the effect of solute structure on the retention. These are: the total dipole moment, the mean polarizability, the anisotropy of polarizability and a descriptor of hydrogen bonding ability based on the atomic charges on hydrogen bond donor and acceptor chemical functionalities. The proposed nonlinear QSRR model exhibits a high degree of correlation between observed and computed retention factors and a good predictive performance in wide range of mobile phase composition (40-65%, v/v acetonitrile) that supports its application for the prediction of the chromatographic behaviour of unknown pesticides. A multilinear regression model based on the same six descriptors shows a significantly worse predictive capability.

Gradient Scouting in Reversed-Phase HPLC Revisited

Science.gov (United States)

Alcazar, A.; Jurado, J. M.; Gonzalez, A. G.

2011-01-01

Gradient scouting is the best way to decide the most suitable elution mode in reversed-phase high-performance liquid chromatography (RP-HPLC). A simple rule for this decision involves the evaluation of the ratio [delta]t/t[subscript G] (where [delta]t is the difference in the retention time between the last and the first peak and t[subscript G] is…

Determination of free urinary cortisol in cushing's syndrome using reversed-phase high performance liquid chromatography

Directory of Open Access Journals (Sweden)

Eduardo Kinio Sugawara

2010-01-01

Full Text Available Determination of free urinary cortisol is a test of choice in the diagnosis of Cushing's syndrome. In this study, cortisol was quantified using reversed-phase high-performance liquid chromatography (RP-HPLC in urine samples previously extracted with ether and using triamcinolone acetonide as internal standard (IS. A BDS-Hypersil-C18® column, water-acetonitrile (72:28; v/v, with a flow rate of 1.0 mL/min and detection at 243 nm were used. This method showed to be both effective and efficient, with sensitivity and linearity ranging from 2.50 to 150 μg/L, and can be used in substitution to the radioimmunoassay technique within this concentration range.

Facile preparation of an alternating copolymer-based high molecular shape-selective organic phase for reversed-phase liquid chromatography.

Science.gov (United States)

Mallik, Abul K; Noguchi, Hiroki; Rahman, Mohammed Mizanur; Takafuji, Makoto; Ihara, Hirotaka

2018-06-22

The synthesis of a new alternating copolymer-grafted silica phase is described for the separation of shape-constrained isomers of polycyclic aromatic hydrocarbons (PAHs) and tocopherols in reversed-phase high-performance liquid chromatography (RP-HPLC). Telomerization of the monomers (octadecyl acrylate and N-methylmaleimide) was carried out with a silane coupling agent; 3-mercaptopropyltrimethoxysilane (MPS), and the telomer (T) was grafted onto porous silica surface to prepare the alternating copolymer-grafted silica phase (Sil-alt-T). The new hybrid material was characterized by elemental analyses, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, and solid-state 13 C and 29 Si cross-polarization magic-angle spinning (CP/MAS) NMR spectroscopy. The results of 13 C CP/MAS NMR demonstrated that the alkyl chains of the grafted polymers in Sil-alt-T remained disordered, amorphous, and mobile represented by gauche conformational form. Separation abilities and molecular-shape selectivities of the prepared organic phase were evaluated by the separation of PAHs isomers and Standard Reference Material 869b, Column Selectivity Test Mixture for Liquid Chromatography, respectively and compared with commercially available octadecylsilylated silica (ODS) and C 30 columns as well as previously reported alternating copolymer-based column. The effectiveness of this phase is also demonstrated by the separation of tocopherol isomers. Oriented functional groups along the polymer main chains and cavity formations are investigated to be the driving force for better separation with multiple-interactions with the solutes. One of the advantages of the Sil-alt-T phase to that of the previously reported phase is the synthesis of the telomer first and then immobilized onto silica surface. In this case, the telomer was characterized easily with simple spectroscopic techniques and the molecular mass and polydispersity index of the telomer were determined by size exclusion

Analysis of Theobromine and Related Compounds by Reversed Phase High-Performance Liquid Chromatography with Ultraviolet Detection: An Update (1992–2011

Directory of Open Access Journals (Sweden)

Sandra Aparecida de Assis

2011-01-01

Full Text Available Theobromine and its related compounds, such as caffeine and theophylline, are secondary metabolites that belong to the alkaloids and have economic and cultural importance. These alkaloids have demonstrated stimulatory effects on the central nervous, gastrointestinal, cardiovascular, renal and respiratory systems, resulting in 'energy arousal', increased motivation to work, increased alertness and increased cognitive function. Several analytical methods have been used to analyse these compounds, but reversed phase high-performance liquid chromatography (RP-HPLC is the most commonly applied because of its efficiency, sensitivity, specificity and speed. This review describes the analyses of theobromine-related compounds by RP-HPLC with ultraviolet detection (UV in four sources: food, beverages, biological fluids and plants. Many RP-HPLC methods have been developed and optimized for the detection and quantification of these natural compounds. Elution under isocratic conditions is the most frequent method, with a water, methanol and acetonitrile mixture modified with acetic, phosphoric or formic acid as the mobile phase. For xanthine analysis, the use of reversed phase high-performance liquid chromatography with an ultraviolet/diode array detector (UV/DAD is particularly suitable as derivation is not required; it allows the analysis of absorbance at all wavelengths, it is simple and rapid.

[Separation and determination of eight plant hormones by reversed-phase high performance liquid chromatography].

Science.gov (United States)

Fang, N; Hou, S; Shao, X; He, Y; Zhao, G

1998-09-01

In this paper, reversed-phase high performance liquid chromatographic technique was used for the separation and determination of eight plant hormones. Methanol-water-acetic acid system was chosen as the mobile phase. The effects of different separation conditions, such as the methanol and acetic acid concentrations in mobile phase, on the retention behaviours of eight plant hormones in this system were studied. The general trends in retention behaviours could be correlated to the methanol concentration in mobile phase. The experimental results showed that the optimum separation was achieved with following gradient elution condition: 0-3 minutes, 70% (water percentage in mobile phase), 3-13 minutes, 70%-20%, 13-48 minutes, 20%. Benzene was added to be as the internal standard. Under this experimental condition, the eight plant hormones could be separated completely and detected quantitatively at 260 nm within 16 minutes. The calibration curves for the eight compounds gave linearity over a wide range. The correlation coefficients of each components were r(ZT) = 0.9971, r(GAs) = 0.9999, r(K) = 0.9997, r(BA) = 0.9995, r(IAA) = 0.9998, r(IPA) = 0.9982, r(IBA) = 0.9995 and r(NAA) = 0.9995. The method is rapid, simple and efficient. It is a suitable method for the accurate determination of gibberellic acid (GA) and alpha-naphthaleneacetic acid (alpha-NAA) in products for agricultural use.

Surface-bonded ionic liquid stationary phases in high-performance liquid chromatography--a review.

Science.gov (United States)

Pino, Verónica; Afonso, Ana M

2012-02-10

Ionic liquids (ILs) are a class of ionic, nonmolecular solvents which remain in liquid state at temperatures below 100°C. ILs possess a variety of properties including low to negligible vapor pressure, high thermal stability, miscibility with water or a variety of organic solvents, and variable viscosity. IL-modified silica as novel high-performance liquid chromatography (HPLC) stationary phases have attracted considerable attention for their differential behavior and low free-silanol activity. Indeed, around 21 surface-confined ionic liquids (SCIL) stationary phases have been developed in the last six years. Their chromatographic behavior has been studied, and, despite the presence of a positive charge on the stationary phase, they showed considerable promise for the separation of neutral solutes (not only basic analytes), when operated in reversed phase mode. This aspect points to the potential for truly multimodal stationary phases. This review attempts to summarize the state-of-the-art about SCIL phases including their preparation, chromatographic behavior, and analytical performance. Copyright © 2011 Elsevier B.V. All rights reserved.

Development and validation of a reversed phase High Performance ...

African Journals Online (AJOL)

A simple, rapid, accurate and economical isocratic Reversed Phase High Performance Liquid Chromatography (RPHPLC) method was developed, validated and used for the evaluation of content of different brands of paracetamol tablets. The method was validated according to ICH guidelines and may be adopted for the ...

Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

Science.gov (United States)

Martha J.M. Wells; Jerry L. Michael

1987-01-01

Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

Structure-retention and mobile phase-retention relationships for reversed-phase high-performance liquid chromatography of several hydroxythioxanthone derivatives in binary acetonitrile-water mixtures

International Nuclear Information System (INIS)

Amiri, Ali Asghar; Hemmateenejad, Bahram; Safavi, Afsaneh; Sharghi, Hashem; Beni, Ali Reza Salimi; Shamsipur, Mojtaba

2007-01-01

The reversed-phase high-performance liquid chromatographic (RP-HPLC) behavior of some newly synthesized hydroxythioxanthone derivatives using binary acetonitrile-water mixtures as mobile phase has been examined. First, the variation in the retention time of each molecule as a function of mobile phase properties was studied by Kamlet-Taft solvatochromic equations. Then, the influences of molecular structure of the hydroxythioxanthone derivatives on their retention time in various mobile phase mixtures were investigated by quantitative structure-property relationship (QSPR) analysis. Finally, a unified model containing both the molecular structure parameters and mobile phase properties was developed to describe the chromatographic behavior of the systems studied. Among the solvent properties, polarity/polarizability parameter (π * ) and hydrogen-bond basicity (β), and among the solute properties, the most positive local charge (MPC), the sum of positive charges on hydrogen atoms contributing in hydrogen bonding (SPCH) and lipophilicity index (log P) were identified as controlling factors in the RP-HPLC behavior of hydroxythioxanthone derivatives in actonitrile-water binary solvents

Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

2013-07-26

A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals. Copyright © 2013 Elsevier B.V. All rights reserved.

Comprehensive analysis of pharmaceutical products using simultaneous mixed-mode (ion-exchange/reversed-phase) and hydrophilic interaction liquid chromatography.

Science.gov (United States)

Kazarian, Artaches A; Nesterenko, Pavel N; Soisungnoen, Phimpha; Burakham, Rodjana; Srijaranai, Supalax; Paull, Brett

2014-08-01

Liquid chromatographic assays were developed using a mixed-mode column coupled in sequence with a hydrophilic interaction liquid chromatography column to allow the simultaneous comprehensive analysis of inorganic/organic anions and cations, active pharmaceutical ingredients, and excipients (carbohydrates). The approach utilized dual sample injection and valve-mediated column switching and was based upon a single high-performance liquid chromatography gradient pump. The separation consisted of three distinct sequential separation mechanisms, namely, (i) ion-exchange, (ii) mixed-mode interactions under an applied dual gradient (reversed-phase/ion-exchange), and (iii) hydrophilic interaction chromatography. Upon first injection, the Scherzo SS C18 column (Imtakt) provided resolution of inorganic anions and cations under isocratic conditions, followed by a dual organic/salt gradient to elute active pharmaceutical ingredients and their respective organic counterions and potential degradants. At the top of the mixed-mode gradient (high acetonitrile content), the mobile phase flow was switched to a preconditioned hydrophilic interaction liquid chromatography column, and the standard/sample was reinjected for the separation of hydrophilic carbohydrates, some of which are commonly known excipients in drug formulations. The approach afforded reproducible separation and resolution of up to 23 chemically diverse solutes in a single run. The method was applied to investigate the composition of commercial cough syrups (Robitussin®), allowing resolution and determination of inorganic ions, active pharmaceutical ingredients, excipients, and numerous well-resolved unknown peaks. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Study of Separation and Identification of the Active Ingredients in Gardenia jasminoides Ellis Based on a Two-Dimensional Liquid Chromatography by Coupling Reversed Phase Liquid Chromatography and Hydrophilic Interaction Liquid Chromatography.

Science.gov (United States)

Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

2017-01-01

In this paper, by coupling reversed phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), a two-dimensional liquid chromatography system was developed for separation and identification of the active ingredients in Gardenia jasminoides Ellis (GJE). By applying the semi-preparative C18 column as the first dimension and the core-shell column as the second dimension, a total of 896 peaks of GJE were separated. Among the 896 peaks, 16 active ingredients including geniposide, gardenoside, gardoside, etc. were identified by mass spectrometry analysis. The results indicated that the proposed two-dimensional RPLC/HILIC system was an effective method for the analysis of GJE and might hold a high potential to become a useful tool for analysis of other complex mixtures. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Single component, reversible ionic liquids for energy applications

Energy Technology Data Exchange (ETDEWEB)

Vittoria Blasucci; Ryan Hart; Veronica Llopis Mestre; Dominique Julia Hahne; Melissa Burlager; Hillary Huttenhower; Beng Joo Reginald Thio; Pamela Pollet; Charles L. Liotta; Charles A. Eckert [Georgia Institute of Technology, Atlanta, GA (United States). Chemical & Biomolecular Engineering

2010-06-15

Single component, reversible ionic liquids have excellent potential as novel solvents for a variety of energy applications. Our energy industry is faced with many new challenges including increased energy consumption, depleting oil reserves, and increased environmental awareness. We report the use of reversible ionic liquids to solve two energy challenges: extraction of hydrocarbons from contaminated crude oil and carbon capture from power plant flue gas streams. Our reversible solvents are derived from silylated amine molecular liquids which react with carbon dioxide reversibly to form ionic liquids. Here we compare the properties of various silylated amine precursors and their corresponding ionic liquids. We show how the property changes are advantageous in the two aforementioned energy applications. In the case of hydrocarbon purification, we take advantage of the polarity switch between precursor and ionic liquid to enable separations. In carbon capture, our solvents act as dual physical and chemical capture agents for carbon dioxide. Finally, we show the potential economics of scale-up for both processes. 20 refs., 1 fig., 3 tabs.

3D printed titanium micro-bore columns containing polymer monoliths for reversed-phase liquid chromatography.

Science.gov (United States)

Gupta, Vipul; Talebi, Mohammad; Deverell, Jeremy; Sandron, Sara; Nesterenko, Pavel N; Heery, Brendan; Thompson, Fletcher; Beirne, Stephen; Wallace, Gordon G; Paull, Brett

2016-03-03

The potential of 3D selective laser melting (SLM) technology to produce compact, temperature and pressure stable titanium alloy chromatographic columns is explored. A micro bore channel (0.9 mm I.D. × 600 mm long) was produced within a 5 × 30 × 30 mm titanium alloy (Ti-6Al-4V) cuboid, in form of a double handed spiral. A poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) (BuMA-co-EDMA) monolithic stationary phase was thermally polymerised within the channel for application in reversed-phase high-performance liquid chromatography. The prepared monolithic column was applied to the liquid chromatographic separation of intact proteins and peptides. Peak capacities of 69-76 (for 6-8 proteins respectively) were observed during isothermal separation of proteins at 44 °C which were further increased to 73-77 using a thermal step gradient with programmed temperature from 60 °C to 35 °C using an in-house built direct-contact heater/cooler platform based upon matching sized Peltier thermoelectric modules. Rapid temperature gradients were possible due to direct-contact between the planar metal column and the Peltier module, and the high thermal conductivity of the titanium column as compared to a similar stainless steel printed column. The separation of peptides released from a digestion of E.coli was also achieved in less than 35 min with ca. 40 distinguishable peaks at 210 nm. Copyright © 2016 Elsevier B.V. All rights reserved.

Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

NARCIS (Netherlands)

Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

1995-01-01

In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

Photoinduced critical opalescence and reversible all-optical switching in photosensitive liquid crystals

International Nuclear Information System (INIS)

Tabiryan, Nelson V.; Serak, Svetlana V.; Grozhik, Vladimir A.

2003-01-01

We present the results of a study of the critical opalescence that is observed as a result of reversible trans-cis photoisomerization in the vicinity of photoinduced isothermal phase transitions in azobenzene liquid crystals (azo LCs). The opalescence is caused by the generation of randomly oriented microdomains and microdroplets of isotropic phase in the illuminated area of the azo LC. Transformations between the strongly light-scattering nematic phase and the transparent isotropic phase of the azo LC are induced all-optically by combination of green (λ=532 nm) and violet (λ=409 nm) laser beams

Photoinduced critical opalescence and reversible all-optical switching in photosensitive liquid crystals

Science.gov (United States)

Tabiryan, Nelson V.; Serak, Svetlana V.; Grozhik, Vladimir A.

2003-03-01

We present the results of a study of the critical opalescence that is observed as a result of reversible trans-cis photoisomerization in the vicinity of photoinduced isothermal phase transitions in azobenzene liquid crystals (azo LCs). The opalescence is caused by the generation of randomly oriented microdomains and microdroplets of isotropic phase in the illuminated area of the azo LC. Transformations between the strongly light-scattering nematic phase and the transparent isotropic phase of the azo LC are induced all-optically by combination of green (λ=532 nm) and violet (λ=409 nm) laser beams.

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.

Complete separation of racemic p-boronophenylalanine by high performance liquid chromatography with crown ether-coated reversed-phase packings

International Nuclear Information System (INIS)

Yoshino, K.; Mieda, S.; Maruyama, T.; Mori, Y.; Mishima, Y.; Ichihashi, M.

1992-01-01

Since the L-form of p-boronophenylalanine (p-bpa) has been shown to be more efficiently incorporated into melanoma cells than racemic p-bpa separation of racemic p-bpa into its stereoisomers is an important subject. One of the preparative methods used to resolve racemic p-bpa involves the use of α-chymotrypsin. However, there has been a problem in that optical purity of resolved L- or D-p-bpa products was not easily determined. In this paper, the authors describe a method which can be used to confirm the optical purity of b-pba using high performance liquid chromatography (HPLC) with crown ether-coated reversed-phase packings

Analytical method development and validation of simultaneous estimation of rabeprazole, pantoprazole, and itopride by reverse-phase high-performance liquid chromatography

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Senthamil Selvan Perumal

2014-12-01

Full Text Available A simple, selective, rapid, and precise reverse-phase high-performance liquid chromatography (RP-HPLC method for the simultaneous estimation of rabeprazole (RP, pantoprazole (PP, and itopride (IP has been developed. The compounds were well separated on a Phenomenex C18 (Luna column (250 mm × 4.6 mm, dp = 5 μm with C18 guard column (4 mm × 3 mm × 5 μm with a mobile phase consisting of buffer containing 10 mM potassium dihydrogen orthophosphate (adjusted to pH 6.8: acetonitrile (70:30 v/v at a flow rate of 1.0 mL/min and ultraviolet detection at 288 nm. The retention time of RP, PP, and IP were 5.35, 7.92, and 11.16 minutes, respectively. Validation of the proposed method was carried out according to International Conference on Harmonisation (ICH guidelines. Linearity range was obtained for RP, PP, and IP over the concentration range of 2.5–25, 1–30, and 3–35 μg/mL and the r2 values were 0.994, 0.978, and 0.991, respectively. The calculated limit of detection (LOD values were 1, 0.3, and 1 μg/mL and limit of quantitation (LOQ values were 2.5, 1, and 3 μg/mL for RP, PP, and IP correspondingly. Thus, the current study showed that the developed reverse-phase liquid chromatography method is sensitive and selective for the estimation of RP, PP, and IP in combined dosage form.

Analytical method development and validation of simultaneous estimation of rabeprazole, pantoprazole, and itopride by reverse-phase high-performance liquid chromatography.

Science.gov (United States)

Perumal, Senthamil Selvan; Ekambaram, Sanmuga Priya; Raja, Samundeswari

2014-12-01

A simple, selective, rapid, and precise reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of rabeprazole (RP), pantoprazole (PP), and itopride (IP) has been developed. The compounds were well separated on a Phenomenex C 18 (Luna) column (250 mm × 4.6 mm, dp = 5 μm) with C 18 guard column (4 mm × 3 mm × 5 μm) with a mobile phase consisting of buffer containing 10 mM potassium dihydrogen orthophosphate (adjusted to pH 6.8): acetonitrile (70:30 v/v) at a flow rate of 1.0 mL/min and ultraviolet detection at 288 nm. The retention time of RP, PP, and IP were 5.35, 7.92, and 11.16 minutes, respectively. Validation of the proposed method was carried out according to International Conference on Harmonisation (ICH) guidelines. Linearity range was obtained for RP, PP, and IP over the concentration range of 2.5-25, 1-30, and 3-35 μg/mL and the r 2 values were 0.994, 0.978, and 0.991, respectively. The calculated limit of detection (LOD) values were 1, 0.3, and 1 μg/mL and limit of quantitation (LOQ) values were 2.5, 1, and 3 μg/mL for RP, PP, and IP correspondingly. Thus, the current study showed that the developed reverse-phase liquid chromatography method is sensitive and selective for the estimation of RP, PP, and IP in combined dosage form. Copyright © 2014. Published by Elsevier B.V.

Simultaneous determination of 18α-glycyrrhetinic acid and 18β-glycyrrhetinic acid in Glycyrrhiza glabra root by reversed phase high-performance liquid chromatography

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Ambika Chamoli

2016-01-01

Full Text Available Background: The aim of the present research work is to develop a high-performance liquid chromatography (HPLC method for simultaneous analysis of 18α-glycyrrhetinic acid (18α-GA and 18β-GA (18β-GA of Glycyrrhiza glabra. Materials and Methods: About 20 μL aliquots of each 18α-GA and 18β-GA were analyzed using reversed-phase C-18 column. The mobile phase was acetonitrile:tetrahydrofuran:water (10:80:10, v/v/v. The run time was 10 min at flow rate of 1 ml/min. Ultraviolet detection was carried out at 254 nm. Results: 18α-GA and 18β-GA were well resolved in reversed phase C-18 column using mobile phase acetonitrile: tetrahydrofuran: water (10:80:10, v/v/v, pH 7.9. The Rtof 18α-GA and 18β-GA was detected at 2.091 and 2.377 min, respectively. Conclusion: The developed chromatography method could be extended for potential quantification or simultaneous determination of these markers in plant as well as in herbal formulation.

[Determination of acyclovir in mouse plasma and tissues by reversed-phase high performance liquid chromatography].

Science.gov (United States)

Xu, Y; Zhou, S W; Tang, J L; Huang, L Q

2001-11-01

The aim of this study was to establish an high performance liquid chromatographic method for determining acyclovir (ACV) concentration in mouse plasma and tissues. A solution of 0.25 mL 60 g/L perchloric acid and 0.25 mL acetonitrile was added into 0.2 mL plasma or 0.2 g tissues to precipitate proteins. Following centrifugation, the supernatant obtained was injected into a reversed-phase column. Operating conditions were Hypersil ODS column(250 mm x 4.6 mm i.d., 5 microns), methanol-water-acetic acid(1:99:0.5, volume ratio) solution as mobile phase at a flow rate of 1.5 mL/min, UV detection at 252 nm. The detection limit of ACV concentration in plasma was 20 micrograms/L and that in tissues was 50 ng/g. The standard curves for ACV were linear in plasma and homogenate of tissues (r > 0.99). The precision of the method was good and the recoveries of ACV were higher than 97.5%. So this method is rapid, accurate and convenient for determination of ACV concentrations in plasma and tissues.

Utility of reversed phase high performance liquid chromatography for on-line yield determination of radiochemical separations: Studies with cobalt

International Nuclear Information System (INIS)

Subramanian, S.; Woittiez, J.R.W.

1993-01-01

This article indicates the potentials of high performance liquid chromatography (HPLC) as a radiochemical technique for multielement separation of neutron irradiated samples. The focus lies on the convenience to use the detector signal of the eluted components to indicate the chemical yield of the analyte, which has often proved to be a crucial step in radiochemical separations. Two signals have been utilized. The UV signal of the metal-ligand complexes separated by reversed phase HPLC and the radioactive response as a result of sample irradiation of carrier-tracer addition. Change in ratio is discussed between the two signals, if any, for a specific sample. Losses of metal as much as 65% were simulated and corrected using the individual UV response. The method promises improved accuracy for elemental analysis despite losses suffered during the various chemical steps. The procedure omits the necessity of additional analytical steps for yield determination. The present article aims at the chromatographic part of the study. Cobalt as cobalt diethyldithiocarbamate has been used to demonstrate the viability of the concept. The separation was developed on c C18 reverse phase analytical column and optimized on a semi preparative one

Characterization of Isomeric Glycans by Reversed Phase Liquid Chromatography-Electronic Excitation Dissociation Tandem Mass Spectrometry

Science.gov (United States)

Tang, Yang; Wei, Juan; Costello, Catherine E.; Lin, Cheng

2018-04-01

The occurrence of numerous structural isomers in glycans from biological sources presents a severe challenge for structural glycomics. The subtle differences among isomeric structures demand analytical methods that can provide structural details while working efficiently with on-line glycan separation methods. Although liquid chromatography-tandem mass spectrometry (LC-MS/MS) is a powerful tool for mixture analysis, the commonly utilized collision-induced dissociation (CID) method often does not generate a sufficient number of fragments at the MS2 level for comprehensive structural characterization. Here, we studied the electronic excitation dissociation (EED) behaviors of metal-adducted, permethylated glycans, and identified key spectral features that could facilitate both topology and linkage determinations. We developed an EED-based, nanoscale, reversed phase (RP)LC-MS/MS platform, and demonstrated its ability to achieve complete structural elucidation of up to five structural isomers in a single LC-MS/MS analysis. [Figure not available: see fulltext.

Development of anion-exchange/reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry methods for the speciation of bio-available iodine and bromine from edible seaweed.

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Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

2012-05-04

Anion exchange high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry has been novelly applied to assess inorganic (iodide and iodate) and organic (3-iodotyrosine - MIT, and 3,5-diiodotyrosine - DIT) iodine species in a single chromatographic run. The optimized operating conditions (Dionex IonPac AS7, gradient elution with 175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase and flow rates within the 0.5-1.5 mL min(-1) range) have also been used to perform inorganic bromine speciation analysis (bromide and bromate). The developed method has been applied for determining the bio-available contents of iodine and bromine species in dialyzates from edible seaweed. Reverse phase high performance liquid chromatography (Zorbax Eclipse XDB-C8, gradient elution with 0.2% (m/m) acetic acid, and 0.2% (m/m) acetic acid in methanol, as mobile phases, and a constant flow rate of 0.75 mL min(-1)) also hyphenated with inductively coupled plasma-mass spectrometry was used to confirm the presence of organic iodine species (MIT and DIT) in the dialyzates. The verification of the presence of iodinated amino acids (MIT and DIT) in the extracts was also performed by reverse phase high performance liquid chromatography-electrospray ionization-mass spectrometry (LTQ Orbitrap). The developed methods have provided good repeatability (RSD values lower than 10% for both anion exchange and reverse phase separations) and analytical recoveries within the 90-105% range for all cases. The in vitro bio-availability method consisted of a simulated gastric and an intestinal digestion/dialysis (10 kDa molecular weight cut-off - MWCO) two-stage procedure. Iodide and MIT were the main bio-available species quantified, whereas bromide was the major bromine species found in the extracts. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of tropane alkaloids by heart cutting reversed phase - Strong cation exchange two dimensional liquid chromatography.

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Long, Zhen; Zhang, Yanhai; Gamache, Paul; Guo, Zhimou; Steiner, Frank; Du, Nana; Liu, Xiaoda; Jin, Yan; Liu, Xingguo; Liu, Lvye

2018-01-01

Current Chinese Pharmacopoeia (ChP) standards apply liquid extraction combined with one dimensional liquid chromatography (1DLC) method for determining alkaloids in herbal medicines. The complex pretreatments lead to a low analytical efficiency and possible component loss. In this study, a heart cutting reversed phase - strong cation exchange two dimensional liquid chromatography (RP - SCX 2DLC) approach was optimized for simultaneously quantifying tropane alkaloids (anisodine, scopolamine and hyoscyamine) in herbal medicines and herbal medicine tablets without further treatment of the filtered extract. The chromatographic conditions were systematically optimized in terms of column type, mobile phase composition and flow rate. To improve peak capacity and obtain symmetric peak shape of alkaloids, a polar group embedded C18 column combined with chaotropic salts was used in the first dimension. To remove the disturbance of non-alkaloids, achieve unique selectivity and acquire symmetric peak shape of alkaloids, an SCX column combined with phosphate buffer was used in the second dimension. Method validation was performed in terms of linearity, precision (0.54-0.82%), recovery (94.1-105.2%), limit of detection (LOD) and limit of quantification (LOQ) of the three analytes varied between 0.067-0.115mgL -1 and 0.195-0.268mgL -1 , respectively. The method demonstrated superiority over 1DLC method in respect of resolution (less alkaloid co-eluted), sample preparation (no pretreatment procedure) and transfer rate (minimum component loss). The optimized RP - SCX 2DLC approach was subsequently applied to quantify target alkaloids in five herbal medicines and herbal medicine tablets from three different manufactures. The results demonstrated that the developed heart cutting RP - SCX 2DLC approach represented a new, strategically significant methodology for the quality evaluation of tropane alkaloid in related herbal medicines that involve complex chemical matrix. Copyright �

Inulin in Medicinal Plants (IV) : Reversed-Phase High-Performance Liquid Chromatography of Inulin after Acetylation : Molecular-Weight Distribution of Inulin in Medicinal Plants

OpenAIRE

三野, 芳紀; 筒井, 聡美; 太田, 長世; YOSHIKI, MINO; SATOMI, TSUTSUI; NAGAYO, OTA; 大阪薬科大学; 大阪薬科大学; 大阪薬科大学; Osaka College of Pharmacy; Osaka College of Pharmacy; Osaka College of Pharmacy

1985-01-01

Reversed-phase high-performance liquid chromatography coupled with pre-acetylation enabled acculate molecular-weight assay of inulin in medicinal plants to be conducted. The results clearly showed that the molecular-weight distribution of inulin varied depending on the stage of growth: Small molecular weight inulin polymers were detected in large quantity in the earlier growth stage whereas large molecular weight inulin polymers at the flowering and post flowering period.

Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

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Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

2015-05-29

Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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)

Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

Science.gov (United States)

O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

2009-01-01

Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

Analysis of quaternary ammonium and phosphonium ionic liquids by reversed-phase high-performance liquid chromatography with charged aerosol detection and unified calibration.

Science.gov (United States)

Stojanovic, Anja; Lämmerhofer, Michael; Kogelnig, Daniel; Schiesel, Simone; Sturm, Martin; Galanski, Markus; Krachler, Regina; Keppler, Bernhard K; Lindner, Wolfgang

2008-10-31

Several hydrophobic ionic liquids (ILs) based on long-chain aliphatic ammonium- and phosphonium cations and selected aromatic anions were analyzed by reversed-phase high-performance liquid chromatography (RP-HPLC) employing trifluoroacetic acid as ion-pairing additive to the acetonitrile-containing mobile phase and adopting a step-gradient elution mode. The coupling of charged aerosol detection (CAD) for the non-chromophoric aliphatic cations with diode array detection (DAD) for the aromatic anions allowed their simultaneous analysis in a set of new ILs derived from either tricaprylmethylammonium chloride (Aliquat 336) and trihexyltetradecylphosphonium chloride as precursors. Aliquat 336 is a mix of ammonium cations with distinct aliphatic chain lengths. In the course of the studies it turned out that CAD generates an identical detection response for all the distinct aliphatic cations. Due to lack of single component standards of the individual Aliquat 336 cation species, a unified calibration function was established for the quantitative analysis of the quaternary ammonium cations of the ILs. The developed method was validated according to ICH guidelines, which confirmed the validity of the unified calibration. The application of the method revealed molar ratios of cation to anion close to 1 indicating a quantitative exchange of the chloride ions of the precursors by the various aromatic anions in the course of the synthesis of new ILs. Anomalies of CAD observed for the detection of some aromatic anions (thiosalicylate and benzoate) are discussed.

Determination of free formaldehyde in cosmetics containing formaldehyde-releasing preservatives by reversed-phase dispersive liquid-liquid microextraction and liquid chromatography with post-column derivatization.

Science.gov (United States)

Miralles, Pablo; Chisvert, Alberto; Alonso, M José; Hernandorena, Sandra; Salvador, Amparo

2018-03-30

An analytical method for the determination of traces of formaldehyde in cosmetic products containing formaldehyde-releasing preservatives has been developed. The method is based on reversed-phase dispersive liquid-liquid microextraction (RP-DLLME), that allows the extraction of highly polar compounds, followed by liquid chromatography-ultraviolet/visible (LC-UV/vis) determination with post-column derivatization. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the selected conditions, a mixture of 500 μL of acetonitrile (disperser solvent) and 50 μL of water (extraction solvent) was rapidly injected into 5 mL of toluene sample solution. The extracts were injected into the LC-UV/vis system using phosphate buffer 6 mmol L -1 at pH 2 as mobile phase. After chromatographic separation, the eluate merged with a flow stream of pentane-2,4-dione in ammonium acetate solution as derivatizing reagent and passed throughout a post-column reactor at 85 °C in order to derivatize formaldehyde into 3,5-diacetyl-1,4-dihydrolutidine, according to Hantzsch reaction, which was finally measured spectrophotometrically at 407 nm. The method was successfully validated showing good linearity, an enrichment factor of 86 ± 2, limits of detection and quantification of 0.7 and 2.3 ng mL -1 , respectively, and good repeatability (RSD < 9.2%). Finally, the proposed analytical method was applied to the determination of formaldehyde in different commercial cosmetic samples containing formaldehyde-releasing preservatives, such as bronopol, diazolidinyl urea, imidazolidinyl urea, and DMDM hydantoin, with good relative recovery values (91-113%) thus showing that matrix effects were negligible. The good analytical features of the proposed method besides of its simplicity and affordability, make it useful to carry out the quality control of cosmetic products containing formaldehyde-releasing preservatives. Copyright �

Determination of medronic acid by reversed-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Zhao Xiuyan; Wang Xiaojing; Fu Bo; Ye Zhaoyun; Liu Yinli

2012-01-01

An isocratic liquid chromatographic method with evaporative light scattering detection (ELSD) was developed for the determination of medronic acid and its related sub- stances. Volatile pentylamine was used as the ion-pairing agent. Separations were performed on a Symmetry C8 column with an mobile phase of 98 : 2 (V : V) 30 mmol/L pentylamine (pH 5.0, adjusted with acetic acid)-methanol. The mobile phase was delivered at a flow-rate 1.0 mL/min. The method is applicable to the routine analysis and the quality con- trol of medronic acid. (authors)

Determination of caffeine, theobromine, and theophylline in standard reference material 2384, baking chocolate, using reversed-phase liquid chromatography.

Science.gov (United States)

Thomas, Jeanice Brown; Yen, James H; Schantz, Michele M; Porter, Barbara J; Sharpless, Katherine E

2004-06-02

A rapid and selective isocratic reversed-phase liquid chromatographic method has been developed at the National Institute of Standards and Technology to simultaneously measure caffeine, theobromine, and theophylline in a food-matrix standard reference material (SRM) 2384, Baking Chocolate. The method uses isocratic elution with a mobile phase composition (volume fractions) of 10% acetronitrile/90% water (pH adjusted to 2.5 using acetic acid) at a flow rate of 1.5 mL/min with ultraviolet absorbance detection (274 nm). Total elution time for these analytes is less than 15 min. Concentration levels of caffeine, theobromine, and theophylline were measured in single 1-g samples taken from each of eight bars of chocolate over an eight-day period. Samples were defatted with hexane, and beta-hydroxyethyltheophylline was added as the internal standard. The repeatability for the caffeine, theobromine, and theophylline measurements was 5.1, 2.3, and 1.9%, respectively. The limit of quantitation for all analytes was theobromine, and theophylline in SRM 2384.

Liquid phase and supercooled liquid phase welding of bulk metallic glasses

International Nuclear Information System (INIS)

Kawamura, Y.

2004-01-01

Recent progress on welding in bulk metallic glasses (BMGs) has been reviewed. BMGs have been successfully welded to BMGs or crystalline metals by liquid phase welding using explosion, pulse-current and electron-beam methods, and by supercooled liquid phase welding using friction method. Successful welding of the liquid phase methods was due to the high glass-forming ability of the BMGs and the high concentration of welding energy in these methods. In contrast, the supercooled liquid phase welding was successful due to the thermally stable supercooled liquid state of the BMGs and the superplasticity and viscous flow of the supercooled liquid. The successful welding of BMGs to BMGs and crystalline materials is promising for the future development of BMGs as engineering materials

Rapid determination of human globin chains using reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Wan, Jun-Hui; Tian, Pei-Ling; Luo, Wei-Hao; Wu, Bing-Yi; Xiong, Fu; Zhou, Wan-Jun; Wei, Xiang-Cai; Xu, Xiang-Min

2012-07-15

Reversed-phase high-performance liquid chromatography (RP-HPLC) of human globin chains is an important tool for detecting thalassemias and hemoglobin variants. The challenges of this method that limit its clinical application are a long analytical time and complex sample preparation. The aim of this study was to establish a simple, rapid and high-resolution RP-HPLC method for the separation of globin chains in human blood. Red blood cells from newborns and adults were diluted in deionized water and injected directly onto a micro-jupiter C18 reversed-phase column (250 mm × 4.6 mm) with UV detection at 280 nm. Under the conditions of varying pH or the HPLC gradient, the globin chains (pre-β, β, δ, α, (G)γ and (A)γ) were denatured and separated from the heme groups in 12 min with a retention time coefficient of variation (CV) ranging from 0.11 to 1.29% and a peak area CV between 0.32% and 4.86%. Significant differences (P<0.05) among three groups (normal, Hb H and β thalassemia) were found in the area ratio of α/pre-β+β applying the rapid elution procedure, while P≥0.05 was obtained between the normal and α thalassemia silent/trait group. Based on the ANOVA results, receiver operating characteristic (ROC) curve analysis of the δ/β and α/pre-β+β area ratios showed a sensitivity of 100.0%, and a specificity of 100.0% for indicating β thalassemia carriers, and a sensitivity of 96.6% and a specificity of 89.6% for the prediction of hemoglobin H (Hb H) disease. The proposed cut-off was 0.026 of δ/β for β thalassemia carriers and 0.626 of α/pre-β+β for Hb H disease. In addition, abnormal hemoglobin hemoglobin E (Hb E) and Hb Westmead (Hb WS) were successfully identified using this RP-HPLC method. Our experience in developing this RP-HPLC method for the rapid separation of human globin chains could be of use for similar work. Copyright © 2012 Elsevier B.V. All rights reserved.

Versatile ligands for high-performance liquid chromatography: An overview of ionic liquid-functionalized stationary phases.

Science.gov (United States)

Zhang, Mingliang; Mallik, Abul K; Takafuji, Makoto; Ihara, Hirotaka; Qiu, Hongdeng

2015-08-05

Ionic liquids (ILs), a class of unique substances composed purely by cation and anions, are renowned for their fascinating physical and chemical properties, such as negligible volatility, high dissolution power, high thermal stability, tunable structure and miscibility. They are enjoying ever-growing applications in a great diversity of disciplines. IL-modified silica, transforming the merits of ILs into chromatographic advantages, has endowed the development of high-performance liquid chromatography (HPLC) stationary phase with considerable vitality. In the last decade, IL-functionalized silica stationary phases have evolved into a series of branches to accommodate to different HPLC modes. An up-to-date overview of IL-immobilized stationary phases is presented in this review, and divided into five parts according to application mode, i.e., ion-exchange, normal-phase, reversed-phase, hydrophilic interaction and chiral recognition. Specific attention is channeled to synthetic strategies, chromatographic behavior and separation performance of IL-functionalized silica stationary phases. Copyright © 2015 Elsevier B.V. All rights reserved.

Critical indices for reversible gamma-alpha phase transformation in metallic cerium

Science.gov (United States)

Soldatova, E. D.; Tkachenko, T. B.

1980-08-01

Critical indices for cerium have been determined within the framework of the pseudobinary solution theory along the phase equilibrium curve, the critical isotherm, and the critical isobar. The results obtained verify the validity of relationships proposed by Rushbrook (1963), Griffiths (1965), and Coopersmith (1968). It is concluded that reversible gamma-alpha transformation in metallic cerium is a critical-type transformation, and cerium has a critical point on the phase diagram similar to the critical point of the liquid-vapor system.

Determination of the Trans-resveratrol content of Champagne wines by reversed-phase HPLC

Directory of Open Access Journals (Sweden)

Philippe Jeandet

2006-06-01

Full Text Available Levels of trans-resveratrol in Champagne wines were determined by the use of reversed-phase HPLC with UV and fluorometric detection after liquid-liquid extraction with ethyl acetate. Resveratrol concentrations in Champagne wines range from 20 to 77 μg/L except for the Champagne rosé in which resveratrol reaches several hundred micrograms per litre. The resveratrol content of Champagne wines was also shown to decrease with aging on lees.

Simultaneous determination of furfural and its degradation products, furoic acid and maleic acid, in transformer oil by the reversed-phase vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography.

Science.gov (United States)

Wang, Yifan; Li, Haiyan; Yang, Zhen; Zhang, Weijie; Hua, Jia

2017-12-01

To explore why the use of furfural as a transformer oil-paper insulation aging characteristic is problematic in real world application, we developed a method for the simultaneous determination of furfural, furoic acid, and maleic acid in transformer oil by reversed-phase vortex-assisted liquid-liquid microextraction combined with high-performance liquid chromatography. The conditions for the proposed method were optimized, and the obtained extract can be directly analyzed by high-performance liquid chromatography. The detection limits (signal-to-noise ratio = 3) of the method ranged from 1.0 to 4.6 μg/L, the enrichment factors for furfural, furoic acid, maleic acid, and fumaric acid were 4.6, 25.1, 15.6, and 17.5, respectively, and the recovery rates for three analytes (fumaric acid was undetected) range from 82.1 to 106.2%. The contents of furfural, furoic acid, and maleic acid resulted from accelerated aging of transformer insulation oil-paper were measured using the present method for the first time, and the aging samples were analyzed by liquid chromatography with mass spectrometry for the identification of furoic acid and maleic acid in the aging transformer oil samples. Using the optimal method, the target products of samples at different aging time were tracked and measured. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of modafinil in plasma and urine by reversed phase high-performance liquid-chromatography.

Science.gov (United States)

Schwertner, Harvey A; Kong, Suk Bin

2005-03-09

Modafinil (Provigil) is a new wake-promoting drug that is being used for the management of excessive sleepiness in patients with narcolepsy. It has pharmacological properties similar to that of amphetamine, but without some of the side effects associated with amphetamine-like stimulants. Since modafinil has the potential to be abused, accurate drug-screening methods are needed for its analysis. In this study, we developed a high-performance liquid-chromatographic procedure (HPLC) for the quantitative analysis of modafinil in plasma and urine. (Phenylthio)acetic acid was used as an internal standard for the analysis of both plasma and urine. Modafinil was extracted from urine and plasma with ethyl acetate and ethyl acetate-acetic acid (100:1, v/v), respectively, and analyzed on a C18 reverse phase column with methanol-water-acetic acid (500:500:1, v/v) as the mobile phase. Recoveries from urine and plasma were 80.0 and 98.9%, respectively and the limit of quantitation was 0.1 microg/mL at 233 nm. Forty-eight 2-h post-dose urine samples from sham controls and from individuals taking 200 or 400 mg of modafinil were analyzed without knowledge of drug administration. All 16-placebo urine samples and all 32 2-h post-dose urine samples were correctly classified. The analytical procedure is accurate and reproducible and can be used for therapeutic drug monitoring, pharmacokinetic studies, and drug abuse screening.

Modification of encapsulation pressure of reverse micelles in liquid ethane.

Science.gov (United States)

Peterson, Ronald W; Nucci, Nathaniel V; Wand, A Joshua

2011-09-01

Encapsulation within reverse micelles dissolved in low viscosity fluids offers a potential solution to the slow tumbling problem presented by large soluble macromolecules to solution NMR spectroscopy. The reduction in effective macromolecular tumbling is directly dependent upon the viscosity of the solvent. Liquid ethane is of sufficiently low viscosity at pressures below 5000 psi to offer a significant advantage. Unfortunately, the viscosity of liquid ethane shows appreciable pressure dependence. Reverse micelle encapsulation in liquid ethane often requires significantly higher pressures, which obviates the potential advantages offered by liquid ethane over liquid propane. Addition of co-surfactants or co-solvents can be used to manipulate the minimum pressure required to obtain stable, well-behaved solutions of reverse micelles prepared in liquid ethane. A library of potential additives is examined and several candidates suitable for use with encapsulated proteins are described. Copyright © 2011 Elsevier Inc. All rights reserved.

Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

Science.gov (United States)

Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

2015-07-01

Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Attractive interactions between reverse aggregates and phase separation in concentrated malonamide extractant solutions

International Nuclear Information System (INIS)

Erlinger, C.; Belloni, L.; Zemb, T.; Madic, C.

1999-01-01

Using small angle X-ray scattering, conductivity, and phase behavior determination, the authors show that concentrated solutions of malonamide extractants, dimethyldibutyltetradecylmalonamide (DMDBTDMA), are organized in reverse oligomeric aggregates which have many features in common with reverse micelles. The aggregation numbers of these reverse globular aggregates as well as their interaction potential are determined from absolute scattering curves. An attractive interaction is responsible for the demixing of the oil phase when in equilibrium with excess oil. Prediction of conductivity as well as the formation conditions for the third phase is possible using standard liquid theory applied to the extractant aggregates. The interactions, modeled with the sticky sphere model proposed by Baster, are shown to be due to steric interactions resulting from the hydrophobic tails of the extractant molecule and van der Waals forces between the highly polarizable water core of the reverse micelles. The attractive interaction in the oil phase, equilibrated with water, is determined as a function of temperature, extractant molecule concentration, and proton and neodynium(III) cation concentration. It is shown that van der Waals interactions, with an effective Hamaker constant of 3kT, quantitatively explain the behavior of DMDBTDMA in n-dodecane in terms of scattering as well as phase stability limits

Reversed-phase liquid chromatographic profile of free amino acids in strawberry-tree (Arbutus unedo L.) honey.

Science.gov (United States)

Spano, Nadia; Piras, Irene; Ciulu, Marco; Floris, Ignazio; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Sanna, Gavino

2009-01-01

The typical profile of the free amino acids contained in strawberry-tree (Arbutus unedo L.) honey is reported for the first time. An optimized reversed-phase liquid chromatographic (RP-LC) method with phenyl isothiocyanate precolumn derivatization was used. Fourteen free amino acids were identified and quantified in 16 analytical samples. Proline (65.63%) was found to be the most abundant free amino acid, followed by glutamic acid (6.49%), arginine (5.21%), alanine (5.17%), and phenylalanine (4.97%). The total free amino acid content of strawberry-tree honey (average value, 436 mg/kg) was found to be low in comparison to amounts cited in the literature concerning unifloral honeys. The analytical method was optimized and fully validated in terms of detection and quantitation limits, precision (by testing repeatability and reproducibility), linearity, and bias (by means of recovery tests). The acceptability of the validation protocol results was verified using Horwitz's mathematical model and AOAC guidelines.

Rapid Determination of Bile Acids in Bile from Various Mammals by Reversed-Phase Ultra-Fast Liquid Chromatography.

Science.gov (United States)

Si, Gu Leng Ri; Yao, Peng; Shi, Luwen

2015-08-01

A valid and efficient reversed-phase ultra-fast liquid chromatography method was developed for the simultaneous determination of 13 bile acids in the bile of three mammal species, including rat, pig and human gallstone patients. Chromatographic separation was performed with a Shim-pack XR-ODS column, and the mobile phase consisted of acetonitrile and potassium phosphate buffer (pH 2.6) at a flow rate of 0.5 mL min(-1). The linear detection range of most bile acids ranged from 2 to 600 ng µL(-1) with a good correlation coefficient (>0.9995). The precision of each bile acid was bile acids were separated in 15 min with satisfactory resolution, and the total analysis time was 18 min, including equilibration. The method was successfully applied in rapid screening of bile samples from the three mammals. Significant metabolic frameworks of bile acids among various species were observed, whereas considerable quantitative variations in both inter- and intraspecies were also observed, especially for gallstone patients. Our results suggest that detecting the change of bile acid profiles could be applied for the diagnosis of gallstone disease. © Crown copyright 2014.

Mass transfer with complex chemical reactions in gas–liquid systems : two-step reversible reactions with unit stoichiometric and kinetic orders

NARCIS (Netherlands)

Vas Bhat, R.D.; Kuipers, J.A.M.; Versteeg, G.F.

2000-01-01

An absorption model to study gas–liquid mass transfer accompanied by reversible two-step reactions in the liquid phase has been presented. This model has been used to determine mass transfer rates, enhancement factors and concentration profiles over a wide range of process conditions. Although

Rapid separation of lanthanides and actinides on small particle based reverse phase supports

Energy Technology Data Exchange (ETDEWEB)

Datta, A.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R. [Chemistry Group, Indira Gandhi Centre for Atomic Research, Kalpakkam (India)

2010-07-01

This paper presents the results on the use of short columns (3-5 cm long) with small particle size (1.8 {mu}m) for high performance liquid chromatographic separation of individual lanthanides and uranium from plutonium as well as uranium from thorium to achieve rapid separations i.e. separation time as short as 3.6 min for individual lanthanides, 1 min for thorium-uranium and 4.2 min for uranium from plutonium. These advantages can be exploited to significantly reduce analysis time, liquid waste generation as well as dose to operator when radioactive samples are analysed e.g. burn-up determination. In the present work, a dynamic ion-exchange chromatographic separation technique was employed using camphor-10-sulfonic acid (CSA) as the ion-pairing reagent and {alpha}-hydroxy isobutyric acid ({alpha}-HIBA) as the complexing reagent for the isolation of individual lanthanides as well as the separation of uranium from thorium. Uranium was separated from Pu(III) as well as Pu(IV) by reverse phase HPLC technique. The reverse phase HPLC was also investigated for the isolation and quantitative determination of uranium from thorium as well as lanthanide group from uranium. The dynamic ion-exchange technique using small particle support was demonstrated for measuring the concentrations of lanthanide fission products such as La, Ce, Pr, Nd and Sm in the dissolver solution of fast reactor fuel. Similarly, the assay of uranium in the dissolver solution of fast reactor was carried out using reverse phase HPLC technique. The rapid separation technique using reverse phase HPLC was also demonstrated for separation of lanthanides as a group from uranium matrix; samples of LiCl-KCl eutectic salt containing chlorides of lanthanides in uranium matrix (typically 1: 2000) were analysed. (orig.)

Liquid-liquid phase transition in Stillinger-Weber silicon

International Nuclear Information System (INIS)

Beaucage, Philippe; Mousseau, Normand

2005-01-01

It was recently demonstrated that Stillinger-Weber silicon undergoes a liquid-liquid first-order phase transition deep into the supercooled region (Sastry and Angell 2003 Nat. Mater. 2 739). Here we study the effects of perturbations on this phase transition. We show that the order of the liquid-liquid transition changes with negative pressure. We also find that the liquid-liquid transition disappears when the three-body term of the potential is strengthened by as little as 5%. This implies that the details of the potential could affect strongly the nature and even the existence of the liquid-liquid phase

Highly crosslinked polymeric monoliths for reversed-phase capillary liquid chromatography of small molecules.

Science.gov (United States)

Liu, Kun; Tolley, H Dennis; Lee, Milton L

2012-03-02

Seven crosslinking monomers, i.e., 1,3-butanediol dimethacrylate (1,3-BDDMA), 1,4-butanediol dimethacrylate (1,4-BDDMA), neopentyl glycol dimethacrylate (NPGDMA), 1,5-pentanediol dimethacrylate (1,5-PDDMA), 1,6-hexanediol dimethacrylate (1,6-HDDMA), 1,10-decanediol dimethacrylate (1,10-DDDMA), and 1,12-dodecanediol dimethacrylate (1,12-DoDDMA), were used to synthesize highly cross-linked monolithic capillary columns for reversed-phase liquid chromatography (RPLC) of small molecules. Dodecanol and methanol were chosen as "good" and "poor" porogenic solvents, respectively, for these monoliths, and were investigated in detail to provide insight into the selection of porogen concentration using 1,12-DoDDMA. Isocratic elution of alkylbenzenes at a flow rate of 300 nL/min was conducted for all of the monoliths. Gradient elution of alkylbenzenes and alkylparabens provided high resolution separations. Optimized monoliths synthesized from all seven crosslinking monomers showed high permeability. Several of the monoliths demonstrated column efficiencies in excess of 50,000 plates/m. Monoliths with longer alkyl-bridging chains showed very little shrinking or swelling in solvents of different polarities. Column preparation was highly reproducible; the relative standard deviation (RSD) values (n=3) for run-to-run and column-to-column were less than 0.25% and 1.20%, respectively, based on retention times of alkylbenzenes. Copyright © 2012 Elsevier B.V. All rights reserved.

Mass transfer with complex chemical reactions in gas-liquid systems: two-step reversible reactions with unit stoichiometric and kinetic orders

NARCIS (Netherlands)

Vas bhat, R.D.; Kuipers, J.A.M.; Versteeg, Geert

2000-01-01

An absorption model to study gas¿liquid mass transfer accompanied by reversible two-step reactions in the liquid phase has been presented. This model has been used to determine mass transfer rates, enhancement factors and concentration profiles over a wide range of process conditions. Although

Determination of gouty arthritis' biomarkers in human urine using reversed-phase high-performance liquid chromatography

Directory of Open Access Journals (Sweden)

Lei-Wen Xiang

2014-04-01

Full Text Available Creatinine, uric acid, hypoxanthine and xanthine are important diagnostic biomarkers in human urine for gouty arthritis or renal disease diacrisis. A simple method for simultaneous determination of these biomarkers in urine based on reversed-phase high-performance liquid chromatography (RP-HPLC with ultraviolet (UV detector was proposed. After pretreatment by dilution, centrifugation and filtration, the biomarkers in urine samples were separated by ODS-BP column by elution with methanol/50 mM NaH2PO4 buffer solution at pH 5.26 (5:95. Good linearity between peak areas and concentrations of standards was obtained for the biomarkers with correlation coefficients in the range of 0.9957–0.9993. The proposed analytical method has satisfactory repeatability (the recovery of data in a range of creatinine, uric acid, hypoxanthine and xanthine was 93.49–97.90%, 95.38–96.45%, 112.46–115.78% and 90.82–97.13% with standard deviation of <5%, respectively and the limits of detection (LODs, S/N≥3 for creatinine, uric acid, hypoxanthine, and xanthine were 0.010, 0.025, 0.050 and 0.025 mg/L, respectively. The established method was proved to be simple, accurate, sensitive and reliable for the quantitation of gouty arthritis' biomarkers in human urine samples. The ratio of creatinine to uric acid was found to be a possible factor for assessment of gouty arthritis. Keywords: Gouty arthritis, Creatinine, Uric acid, Hypoxanthine, Xanthine, High-performance liquid chromatography

Experimental (solid + liquid) or (liquid + liquid) phase equilibria of (amine + nitrile) binary mixtures

International Nuclear Information System (INIS)

Domanska, Urszula; Marciniak, Malgorzata

2007-01-01

(Solid + liquid) phase diagrams have been determined for (hexylamine, or octylamine, or 1,3-diaminopropane + acetonitrile) mixtures. Simple eutectic systems have been observed in these mixtures. (Liquid + liquid) phase diagrams have been determined for (octylamine, or decylamine + propanenitrile, or + butanenitrile) mixtures. Mixtures with propanenitrile and butanenitrile show immiscibility in the liquid phase with an upper critical solution temperature, UCST. (Solid + liquid) phase diagrams have been correlated using NRTL, NRTL 1, Wilson and UNIQUAC equations. (Liquid + liquid) phase diagrams have been correlated using NRTL equation

Highly selective spectrophotometric determination of trace amounts of vanadium(V) with 2-(8-quinolylazo)-5-N,N-diethylaminophenol by reversed-phase partition liquid chromatography

International Nuclear Information System (INIS)

Hoshino, Hitoshi; Yotsuyanagi, Takao

1982-01-01

A novel reversed-phase partition liquid chromatography-photometric detection system for the determination of trace amounts of vanadium is described. A strongly colored vanadium(V)-2-(8-quinolylazo)-5-N,N-diethylaminophenolato chelate is separated on a μBondapak-CN column using an aqueous acetonitrile mobile phase and is detected at 540 nm(0.02 absorbance unit full-scale). Because the other common cations give no resolved peaks on the chromatogram under the conditions, the determination of vanadium at 5 x 10 -8 to 1 x 10 -6 mol dm -3 level is free from their interferences in case of the total concentration of such cations less than 5 x 10 -5 mol dm -3 (author)

Prediction of Molar Extinction Coefficients of Proteins and Peptides Using UV Absorption of the Constituent Amino Acids at 214 nm To Enable Quantitative Reverse Phase High-Performance Liquid Chromatography-Mass Spectrometry Analysis

NARCIS (Netherlands)

Kuipers, B.J.H.; Gruppen, H.

2007-01-01

The molar extinction coefficients of 20 amino acids and the peptide bond were measured at 214 nm in the presence of acetonitrile and formic acid to enable quantitative comparison of peptides eluting from reversed-phase high-performance liquid chromatography, once identified with mass spectrometry

Rapid determination of hydrophilic phenols in olive oil by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and screen-printed carbon electrodes.

Science.gov (United States)

Fernández, Elena; Vidal, Lorena; Canals, Antonio

2018-05-01

A novel approach is presented to determine hydrophilic phenols in olive oil samples, employing vortex-assisted reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for sample preparation and screen-printed carbon electrodes for voltammetric analysis. The oxidation of oleuropein, hydroxytyrosol, caffeic acid, ferulic acid and tyrosol was investigated, being caffeic acid and tyrosol selected for quantification. A matrix-matching calibration using sunflower oil as analyte-free sample diluted with hexane was employed to compensate matrix effects. Samples were analyzed under optimized RP-DLLME conditions, i.e., extractant phase, 1M HCl; extractant volume, 100µL; extraction time, 2min; centrifugation time, 10min; centrifugation speed, 4000rpm. The working range showed a good linearity between 0.075 and 2.5mgL -1 (r = 0.998, N = 7) for caffeic acid, and between 0.075 and 3mgL -1 (r = 0.999, N = 8) for tyrosol. The methodological limit of detection was empirically established at 0.022mgL -1 for both analytes, which is significantly lower than average contents found in olive oil samples. The repeatability was evaluated at two different spiking levels (i.e., 0.5mgL -1 and 2mgL -1 ) and coefficients of variation ranged from 8% to 11% (n = 5). The applicability of the proposed method was tested in olive oil samples of different quality (i.e., refined olive oil, virgin olive oil and extra virgin olive oil). Relative recoveries varied between 83% and 108% showing negligible matrix effects. Finally, fifteen samples were analyzed by the proposed method and a high correlation with the traditional Folin-Ciocalteu spectrophotometric method was obtained. Thereafter, the concentrations of the fifteen oil samples were employed as input variables in linear discriminant analysis in order to distinguish between olive oils of different quality. Copyright © 2017 Elsevier B.V. All rights reserved.

About the Shape of the Melting Line as a Possible Precursor of a Liquid-Liquid Phase Transition

Science.gov (United States)

Imre, Attila R.; Rzoska, Sylwester J.

Several simple, non-mesogenic liquids can exists in two or more different liquid forms. When the liquid-liquid line, separating two liquid forms, meets the melting line, one can expect some kind of break on the melting line, caused by the different freezing/melting behaviour of the two liquid forms. Unfortunately recently several researchers are using this vein of thinking in reverse; seeing some irregularity on the melting line, they will expect a break and the appearance of a liquid-liquid line. In this short paper, we are going to show, that in the case of the high-pressure nitrogen studied recently by Mukherjee and Boehler, the high-pressure data can be easily described by a smooth, break-free function, the modified Simon-Glatzel equation. In this way, the break, suggested by them and consequently the suggested appearance of a new liquid phase of the nitrogen might be artefacts.

Reversible temperature regulation of electrical and thermal conductivity using liquid-solid phase transitions.

Science.gov (United States)

Zheng, Ruiting; Gao, Jinwei; Wang, Jianjian; Chen, Gang

2011-01-01

Reversible temperature tuning of electrical and thermal conductivities of materials is of interest for many applications, including seasonal regulation of building temperature, thermal storage and sensors. Here we introduce a general strategy to achieve large contrasts in electrical and thermal conductivities using first-order phase transitions in percolated composite materials. Internal stress generated during a phase transition modulates the electrical and thermal contact resistances, leading to large contrasts in the electrical and thermal conductivities at the phase transition temperature. With graphite/hexadecane suspensions, the electrical conductivity changes 2 orders of magnitude and the thermal conductivity varies up to 3.2 times near 18 °C. The generality of the approach is also demonstrated in other materials such as graphite/water and carbon nanotube/hexadecane suspensions.

Highly sensitive reversed-phase high-performance liquid chromatography assay for the detection of Tamm-Horsfall protein in human urine.

Science.gov (United States)

Akimoto, Masaru; Hokazono, Eisaku; Ota, Eri; Tateishi, Takiko; Kayamori, Yuzo

2016-01-01

Tamm-Horsfall protein (also known as uromodulin) is the most abundant urinary protein in healthy individuals. Since initially characterized by Tamm and Horsfall, the amount of urinary excretion and structural mutations of Tamm-Horsfall protein is associated with kidney diseases. However, currently available assays for Tamm-Horsfall protein, which are mainly enzyme-linked immunosorbent assay-based, suffer from poor reproducibility and might give false negative results. We developed a novel, quantitative assay for Tamm-Horsfall protein using reversed-phase high-performance liquid chromatography. A precipitation pretreatment avoided urine matrix interference and excessive sample dilution. High-performance liquid chromatography optimization based on polarity allowed excellent separation of Tamm-Horsfall protein from other major urine components. Our method exhibited high precision (based on the relative standard deviations of intraday [≤2.77%] and interday [≤5.35%] repetitions). The Tamm-Horsfall protein recovery rate was 100.0-104.2%. The mean Tamm-Horsfall protein concentration in 25 healthy individuals was 31.6 ± 18.8 mg/g creatinine. There was a strong correlation between data obtained by high-performance liquid chromatography and enzyme-linked immunosorbent assay (r = 0.906), but enzyme-linked immunosorbent assay values tended to be lower than high-performance liquid chromatography values at low Tamm-Horsfall protein concentrations. The high sensitivity and reproducibility of our Tamm-Horsfall protein assay will reduce the number of false negative results of the sample compared with enzyme-linked immunosorbent assay. Moreover, our method is superior to other high-performance liquid chromatography methods, and a simple protocol will facilitate further research on the physiological role of Tamm-Horsfall protein. © The Author(s) 2015.

Reversed-phase thin-layer chromatography of homologs of Antimycin-A and related derivatives

Science.gov (United States)

Abidi, Sharon L.

1989-01-01

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.

Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

Science.gov (United States)

Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

2016-04-01

Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

Determination of organic and inorganic mercury species in Sungai Kinta, Perak by reversed-phase high performance liquid chromatography (HPLC) on-line coupled with ICP-MS

International Nuclear Information System (INIS)

Norshidah Baharuddin; Norashikin Saim; Rozita Osman; Sharifuddin Mohd Zain

2012-01-01

This paper describes a simple method for mercury speciation in river water samples of Sungai Kinta, Perak. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ ICP-MS). Separation of mercury species was accomplished within 6 minutes on an AQ C18 4.6 mm i.d x 150 mm, 5 μm reversed phase column with 0.1 % (w/ v) L-cysteine as mobile phase. Under the optimum instrumental conditions, recoveries of 101-104 % for MeHg + and 96 - 104 % for Hg 2+ were obtained with experimental detection limits of 1ngL -1 for inorganic mercury and 1.5 μgL -1 for organic mercury. (author)

Analytical Method Development and Validation for the Simultaneous Estimation of Abacavir and Lamivudine by Reversed-phase High-performance Liquid Chromatography in Bulk and Tablet Dosage Forms.

Science.gov (United States)

Raees Ahmad, Sufiyan Ahmad; Patil, Lalit; Mohammed Usman, Mohammed Rageeb; Imran, Mohammad; Akhtar, Rashid

2018-01-01

A simple rapid, accurate, precise, and reproducible validated reverse phase high performance liquid chromatography (HPLC) method was developed for the determination of Abacavir (ABAC) and Lamivudine (LAMI) in bulk and tablet dosage forms. The quantification was carried out using Symmetry Premsil C18 (250 mm × 4.6 mm, 5 μm) column run in isocratic way using mobile phase comprising methanol: water (0.05% orthophosphoric acid with pH 3) 83:17 v/v and a detection wavelength of 245 nm and injection volume of 20 μl, with a flow rate of 1 ml/min. In the developed method, the retention times of ABAC and LAMI were found to be 3.5 min and 7.4 min, respectively. The method was validated in terms of linearity, precision, accuracy, limits of detection, limits of quantitation, and robustness in accordance with the International Conference on Harmonization guidelines. The assay of the proposed method was found to be 99% - 101%. The recovery studies were also carried out and mean % recovery was found to be 99% - 101%. The % relative standard deviation from reproducibility was found to be performance liquid chromatography, UV: Ultraviolet, ICH: International Conference on Harmonization, ABAC: Abacavir, LAMI: Lamivudine, HIV: Human immunodeficiency virus, AIDS: Acquired immunodeficiency syndrome, NRTI: Nucleoside reverse transcriptase inhibitors, ARV: Antiretroviral, RSD: Relative standard deviation, RT: Retention time, SD: Standard deviation.

[[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

Science.gov (United States)

Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

2014-09-01

Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

Determination of Efavirenz in Human Dried Blood Spots by Reversed-Phase High Performance Liquid Chromatography with UV Detection

Science.gov (United States)

Hoffman, Justin T; Rossi, Steven S; Espina-Quinto, Rowena; Letendre, Scott; Capparelli, Edmund V

2013-01-01

Background Previously published methods for determination of efavirenz (EFV) in human dried blood spots (DBS) employ costly and complex liquid chromatography/mass spectrometry. We describe the validation and evaluation of a simple and inexpensive high-performance liquid chromatography (HPLC) method for EFV quantification in human DBS and dried plasma spots (DPS), using ultraviolet (UV) detection appropriate for resource-limited settings. Methods 100μl of heparinized whole blood or plasma were spotted onto blood collection cards, dried, punched, and eluted. Eluates are injected onto a C-18 reversed phase HPLC column. EFV is separated isocratically using a potassium phosphate and ACN mobile phase. UV detection is at 245nm. Quantitation is by use of external calibration standards. Following validation, the method was evaluated using whole blood and plasma from HIV-positive patients undergoing EFV therapy. Results Mean recovery of drug from dried blood spots is 91.5%. The method is linear over the validated concentration range of 0.3125 – 20.0μg/mL. A good correlation (Spearman r=0.96) between paired plasma and DBS EFV concentrations from the clinical samples was observed, and hematocrit level was not found to be a significant determinant of the EFV DBS level. The mean observed CDBS/Cplasma ratio was 0.68. A good correlation (Spearman r=0.96) between paired plasma and DPS EFV concentrations from the clinical samples was observed. The mean percent deviation of DPS samples from plasma samples is 1.68%. Conclusions Dried whole blood spot or dried plasma spot sampling is well suited for monitoring EFV therapy in resource limited settings, particularly when high sensitivity is not essential. PMID:23503446

Development of a perfusion reversed-phase high performance liquid chromatography method for the characterisation of maize products using multivariate analysis.

Science.gov (United States)

Rodriguez-Nogales, J M; Garcia, M C; Marina, M L

2006-02-03

A perfusion reversed-phase high performance liquid chromatography (RP-HPLC) method has been designed to allow rapid (3.4 min) separations of maize proteins with high resolution. Several factors, such as extraction conditions, temperature, detection wavelength and type and concentration of ion-pairing agent were optimised. A fine optimisation of the gradient elution was also performed by applying experimental design. Commercial maize products for human consumption (flours, precocked flours, fried snacks and extruded snacks) were characterised for the first time by perfusion RP-HPLC and their chromatographic profiles allowed a differentiation among products relating the different technological process used for their preparation. Furthermore, applying discriminant analysis makes it possible to group the samples according with the technological process suffered by maize products, obtaining a good prediction in 92% of the samples.

Rapid Development and Validation of Improved Reversed-Phase High-performance Liquid Chromatography Method for the Quantification of Mangiferin, a Polyphenol Xanthone Glycoside in Mangifera indica.

Science.gov (United States)

Naveen, P; Lingaraju, H B; Prasad, K Shyam

2017-01-01

Mangiferin, a polyphenolic xanthone glycoside from Mangifera indica , is used as traditional medicine for the treatment of numerous diseases. The present study was aimed to develop and validate a reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of mangiferin from the bark extract of M. indica . RP-HPLC analysis was performed by isocratic elution with a low-pressure gradient using 0.1% formic acid: acetonitrile (87:13) as a mobile phase with a flow rate of 1.5 ml/min. The separation was done at 26°C using a Kinetex XB-C18 column as stationary phase and the detection wavelength at 256 nm. The proposed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification, and robustness by the International Conference on Harmonisation guidelines. In linearity, the excellent correlation coefficient more than 0.999 indicated good fitting of the curve and also good linearity. The intra- and inter-day precision showed high reliability and reproducibility of the method. The recovery values at three different levels (50%, 100%, and 150%) of spiked samples were found to be 100.47, 100.89, and 100.99, respectively, and low standard deviation value high accuracy of the method. In robustness, the results remain unaffected by small variation in the analytical parameters, which shows the robustness of the method. Liquid chromatography-mass spectrometry analysis confirmed the presence of mangiferin with M/Z value of 421. The assay developed by HPLC method is a simple, rapid, and reliable for the determination of mangiferin from M. indica . The present study was intended to develop and validate an RP-HPLC method for the quantification of mangiferin from the bark extract of M. indica . The developed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification and robustness by International Conference on Harmonization guidelines. This study proved that the developed

Treatment of low-level radioactive waste liquid by reverse osmosis

International Nuclear Information System (INIS)

Buckley, L.P.; Sen Gupta, S.K.; Slade, J.A.

1995-01-01

The processing of low-level radioactive waste (LLRW) liquids that result from operation of nuclear power plants with reverse osmosis systems is not common practice. A demonstration facility is operating at Chalk River Laboratories (of Atomic Energy of Canada Limited), processing much of the LLRW liquids generated at the site from a multitude of radioactive facilities, ranging from isotope production through decontamination operations and including chemical laboratory drains. The reverse osmosis system comprises two treatment steps--spiral wound reverse osmosis followed by tubular reverse osmosis--to achieve an average volume reduction factor of 30:1 and a removal efficiency in excess of 99% for most radioactive and chemical species. The separation allows the clean effluent to be discharged without further treatment. The concentrated waste stream of 3 wt% total solids is further processed to generate a solid product. The typical lifetimes of the membranes have been nearly 4000 hours, and replacement was required based on increased pressure drops and irreversible loss of permeate flux. Four years of operating experience with the reverse osmosis system, to demonstrate its practicality and to observe and record its efficiency, maintenance requirements and effectiveness, have proven it to be viable for volume reduction and concentration of LLRW liquids generated from nuclear-power-plant operations

Solvation Dynamics in Different Phases of the Lyotropic Liquid Crystalline System.

Science.gov (United States)

Roy, Bibhisan; Satpathi, Sagar; Gavvala, Krishna; Koninti, Raj Kumar; Hazra, Partha

2015-09-03

Reverse hexagonal (HII) liquid crystalline material based on glycerol monooleate (GMO) is considered as a potential carrier for drugs and other important biomolecules due to its thermotropic phase change and excellent morphology. In this work, the dynamics of encapsulated water, which plays important role in stabilization and formation of reverse hexagonal mesophase, has been investigated by time dependent Stokes shift method using Coumarin-343 as a solvation probe. The formation of the reverse hexagonal mesophase (HII) and transformation to the L2 phase have been monitored using small-angle X-ray scattering and polarized light microscopy experiments. REES studies suggest the existence of different polar regions in both HII and L2 systems. The solvation dynamics study inside the reverse hexagonal (HII) phase reveals the existence of two different types of water molecules exhibiting dynamics on a 120-900 ps time scale. The estimated diffusion coefficients of both types of water molecules obtained from the observed dynamics are in good agreement with the measured diffusion coefficient collected from the NMR study. The calculated activation energy is found to be 2.05 kcal/mol, which is associated with coupled rotational-translational water relaxation dynamics upon the transition from "bound" to "quasi-free" state. The observed ∼2 ns faster dynamics of the L2 phase compared to the HII phase may be associated with both the phase transformation as well as thermotropic effect on the relaxation process. Microviscosities calculated from time-resolved anisotropy studies infer that the interface is almost ∼22 times higher viscous than the central part of the cylinder. Overall, our results reveal the unique dynamical features of water inside the cylinder of reverse hexagonal and inverse micellar phases.

Investigation of folic acid stability in fortified instant noodles by use of capillary electrophoresis and reversed-phase high performance liquid chromatography.

Science.gov (United States)

Hau Fung Cheung, Rodney; Morrison, Paul D; Small, Darryl M; Marriott, Philip J

2008-12-05

A single enzyme treatment with alpha-amylase, prior to the quantification of added folic acid (FA) in fortified instant fried Asian noodles with analysis performed by capillary zone electrophoresis (CZE) and reversed-phase high performance liquid chromatography (RP-HPLC) with UV detection, is described. The method was validated and optimized for capillary electrophoresis (CE) with separation achieved using a 8 mM phosphate-12 mM borate run buffer with 5% MeOH at pH 9.5. FA was well separated from matrix components with nicotinic acid (NA) employed as an internal standard. In a comparative study, separation of FA was performed using HPLC with a mobile phase consisting of 27% MeOH (v/v) in aqueous potassium phosphate buffer (3.5 mM KH(2)PO(4) and 3.2 mM K(2)HPO(4)), pH 8.5, and containing 5 mM tetrabutylammonium dihydrogen phosphate as an ion-pairing agent. For both methods, excellent results were obtained for various analytical parameters including linearity, accuracy and precision. The limit of detection was calculated to be 2.2 mg/L for CE without sample stacking and 0.10 mg/L with high performance liquid chromatography (HPLC). Sample extraction involved homogenization and enzymatic extraction with alpha-amylase. Results indicated that FA was stable during four main stages of instant fried noodle manufacturing (dough crumbs, cut sheets, steaming and frying).

Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Yanes, Enrique G.; Miller-Ihli, Nancy J.

2004-01-01

Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories

Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

Science.gov (United States)

Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

2016-02-01

A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

Offline solid-phase extraction for preconcentration of pharmaceuticals and personal care products in environmental water and their simultaneous determination using the reversed phase high-performance liquid chromatography method.

Science.gov (United States)

G Archana; Dhodapkar, Rita; Kumar, Anupama

2016-09-01

The present study reports a precise and simple offline solid-phase extraction (SPE) coupled with reversed-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous determination of five representative and commonly present pharmaceuticals and personal care products (PPCPs), a new class of emerging pollutants in the aquatic environment. The target list of analytes including ciprofloxacin, acetaminophen, caffeine benzophenone and irgasan were separated by a simple HPLC method. The column used was a reversed-phase C18 column, and the mobile phase was 1 % acetic acid and methanol (20:80 v/v) under isocratic conditions, at a flow rate of 1 mL min(-1). The analytes were separated and detected within 15 min using the photodiode array detector (PDA). The linearity of the calibration curves were obtained with correlation coefficients 0.98-0.99.The limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and ruggedness demonstrated the reproducibility, specificity and sensitivity of the developed method. Prior to the analysis, the SPE was performed using a C18 cartridge to preconcentrate the targeted analytes from the environmental water samples. The developed method was applied to evaluate and fingerprint PPCPs in sewage collected from a residential engineering college campus, polluted water bodies such as Nag river and Pili river and the influent and effluent samples from a sewage treatment plant (STP) situated at Nagpur city, in the peak summer season. This method is useful for estimation of pollutants present in microquantities in the surface water bodies and treated sewage as compared to nanolevel pollutants detected by mass spectrometry (MS) detectors.

Quantitative determination of reserpine, ajmaline, and ajmalicine in Rauvolfia serpentina by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Srivastava, A; Tripathi, A K; Pandey, R; Verma, R K; Gupta, M M

2006-10-01

A sensitive and reproducible reversed-phase high-performance liquid chromatography (HPLC) method using photodiode array detection is established for the simultaneous quantitation of important root alkaloids of Rauvolfia serpentina, namely, reserpine, ajmaline, and ajmalicine. A Chromolith Performance RP-18e column (100 x 4.6-mm i.d.) and a binary gradient mobile phase composed of 0.01 M (pH 3.5) phosphate buffer (NaH(2)PO(4)) containing 0.5% glacial acetic acid and acetonitrile are used. Analysis is run at a flow rate of 1.0 mL/min with the detector operated at a wavelength of 254 nm. The calibration curves are linear over a concentration range of 1-20 microg/mL (r = 1.000) for all the alkaloids. The various other aspects of analysis (i.e., peak purity, similarity, recovery, and repeatability) are also validated. For the three components, the recoveries are found to be 98.27%, 97.03%, and 98.38%, respectively. The limits of detection are 6, 4, and 8 microg/mL for ajmaline, ajmalicine, and reserpine, respectively, and the limits of quantitation are 19, 12, and 23 microg/mL for ajmaline, ajmalicine, and reserpine, respectively. The developed method is simple, reproducible, and easy to operate. It is useful for the evaluation of R. serpentina.

Reversible physical absorption of SO2 by ionic liquids

DEFF Research Database (Denmark)

Huang, Jun; Riisager, Anders; Fehrmann, Rasmus

2006-01-01

Ionic liquids can reversibly absorb large amounts of molecular SO2 gas under ambient conditions with the gas captured in a restricted configuration, possibly allowing SO2 to probe the internal cavity structures in ionic liquids besides being useful for SO2 removal in pollution control....

Towards a physical interpretation of third phase formation in liquid-liquid extraction. Application to the Diamex process for the treatment of high radioactive nuclear wastes; Vers une interpretation physique des phenomenes de troisieme phase en extraction liquide-liquide. Application au procede Diamex de traitement des effluents radioactifs de haute activite

Energy Technology Data Exchange (ETDEWEB)

Verdier-Erlinger, C

1998-07-24

Using SAXS, conductivity and phase behaviour determination we show that concentrated solutions of extractants are organised in reverse oligomeric aggregates which have many features in common with reverse micelles. The aggregation numbers of these reverse globular aggregates as well as their interaction potential are determined experimentally. The sticky sphere interaction is responsible for the de-mixing on the oil phase when in equilibrium with excess oil. Prediction of conductivity as well as formation condition for the third phase is possible using standard liquid theory applied to the reverse micelles. The attractive interaction, modeled with the sticky sphere model proposed by Baxter, is the balance of steric stabilisation introduced by the hydrophobic tails of the extracting molecule and the Van der Waals forces between the highly polarizable water core of the reverse molecule concentration, number of carbon atoms of aliphatic solvents, as well as proton and Neodymium cation concentration. It is shown that van der Waals interactions with a Hamaker constant of 2.5 kT explains the behaviour of DMDBTDMA in dodecane. (author) 184 refs.

Reversed phase liquid chromatography with UV absorbance and flame ionization detection using a water mobile phase and a cyano propyl stationary phase Analysis of alcohols and chlorinated hydrocarbons.

Science.gov (United States)

Quigley, W W; Ecker, S T; Vahey, P G; Synovec, R E

1999-10-01

The development of liquid chromatography with a commercially available cyano propyl stationary phase and a 100% water mobile phase is reported. Separations were performed at ambient temperature, simplifying instrumental requirements. Excellent separation efficiency using a water mobile phase was achieved, for example N=18 800, or 75 200 m(-1), was obtained for resorcinol, at a retention factor of k'=4.88 (retention time of 9.55 min at 1 ml min(-1) for a 25 cmx4.6 mm i.d. column, packed with 5 mum diameter particles with the cyano propyl stationary phase). A separation via reversed phase liquid chromatography (RP-LC) with a 100% water mobile phase of six phenols and related compounds was compared to a separation of the same compounds by traditional RP-LC, using octadecylsilane (ODS), i.e. C18, bound to silica and an aqueous mobile phase modified with acetonitrile. Nearly identical analysis time was achieved for the separation of six phenols and related compounds using the cyano propyl stationary phase with a 100% water mobile phase, as compared to traditional RP-LC requiring a relatively large fraction of organic solvent modifier in the mobile phase (25% acetonitrile:75% water). Additional understanding of the retention mechanism with the 100% water mobile phase was obtained by relating measured retention factors of aliphatic alcohols, phenols and related compounds, and chlorinated hydrocarbons to their octanol:water partition coefficients. The retention mechanism is found to be consistent with a RP-LC mechanism coupled with an additional retention effect due to residual hydroxyl groups on the cyano propyl stationary phase. Advantages due to a 100% water mobile phase for the chemical analysis of alcohol mixtures and chlorinated hydrocarbons are reported. By placing an absorbance detector in-series and preceding a novel drop interface to a flame ionization detector (FID), selective detection of a separated mixture of phenols and related compounds and aliphatic

Measurements of liquid-phase turbulence in gas–liquid two-phase flows using particle image velocimetry

International Nuclear Information System (INIS)

Zhou, Xinquan; Doup, Benjamin; Sun, Xiaodong

2013-01-01

Liquid-phase turbulence measurements were performed in an air–water two-phase flow loop with a circular test section of 50 mm inner diameter using a particle image velocimetry (PIV) system. An optical phase separation method-–planar laser-induced fluorescence (PLIF) technique—which uses fluorescent particles and an optical filtration technique, was employed to separate the signals of the fluorescent seeding particles from those due to bubbles and other noises. An image pre-processing scheme was applied to the raw PIV images to remove the noise residuals that are not removed by the PLIF technique. In addition, four-sensor conductivity probes were adopted to measure the radial distribution of the void fraction. Two benchmark tests were performed: the first was a comparison of the PIV measurement results with those of similar flow conditions using thermal anemometry from previous studies; the second quantitatively compared the superficial liquid velocities calculated from the local liquid velocity and void fraction measurements with the global liquid flow rate measurements. The differences of the superficial liquid velocity obtained from the two measurements were bounded within ±7% for single-phase flows and two-phase bubbly flows with the area-average void fraction up to 18%. Furthermore, a preliminary uncertainty analysis was conducted to investigate the accuracy of the two-phase PIV measurements. The systematic uncertainties due to the circular pipe curvature effects, bubble surface reflection effects and other potential uncertainty sources of the PIV measurements were discussed. The purpose of this work is to facilitate the development of a measurement technique (PIV-PLIF) combined with image pre-processing for the liquid-phase turbulence in gas–liquid two-phase flows of relatively high void fractions. The high-resolution data set can be used to more thoroughly understand two-phase flow behavior, develop liquid-phase turbulence models, and assess high

Two complementary reversed-phase separations for comprehensive coverage of the semipolar and nonpolar metabolome.

Science.gov (United States)

Naser, Fuad J; Mahieu, Nathaniel G; Wang, Lingjue; Spalding, Jonathan L; Johnson, Stephen L; Patti, Gary J

2018-02-01

Although it is common in untargeted metabolomics to apply reversed-phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC) methods that have been systematically optimized for lipids and central carbon metabolites, here we show that these established protocols provide poor coverage of semipolar metabolites because of inadequate retention. Our objective was to develop an RPLC approach that improved detection of these metabolites without sacrificing lipid coverage. We initially evaluated columns recently released by Waters under the CORTECS line by analyzing 47 small-molecule standards that evenly span the nonpolar and semipolar ranges. An RPLC method commonly used in untargeted metabolomics was considered a benchmarking reference. We found that highly nonpolar and semipolar metabolites cannot be reliably profiled with any single method because of retention and solubility limitations of the injection solvent. Instead, we optimized a multiplexed approach using the CORTECS T3 column to analyze semipolar compounds and the CORTECS C 8 column to analyze lipids. Strikingly, we determined that combining these methods allowed detection of 41 of the total 47 standards, whereas our reference RPLC method detected only 10 of the 47 standards. We then applied credentialing to compare method performance at the comprehensive scale. The tandem method showed more than a fivefold increase in credentialing coverage relative to our RPLC benchmark. Our results demonstrate that comprehensive coverage of metabolites amenable to reversed-phase separation necessitates two reconstitution solvents and chromatographic methods. Thus, we suggest complementing HILIC methods with a dual T3 and C 8 RPLC approach to increase coverage of semipolar metabolites and lipids for untargeted metabolomics. Graphical abstract Analysis of semipolar and nonpolar metabolites necessitates two reversed-phase chromatography (RPLC) methods, which extend metabolome coverage more

Separation and characterization of chemical constituents in Ginkgo biloba extract by off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography coupled with quadrupole-time of flight mass spectrometry.

Science.gov (United States)

Ji, Shuai; He, Dan-Dan; Wang, Tian-Yun; Han, Jie; Li, Zheng; Du, Yan; Zou, Jia-Hui; Guo, Meng-Zhe; Tang, Dao-Quan

2017-11-30

Ginkgo biloba extract (GBE), derived from the leaves of Ginkgo biloba L., is one of the most widely used traditional Chinese medicines worldwide. Due to high structural diversity and low abundance of chemical constituents in GBE, conventional reversed-phase liquid chromatography has limited power to meet the needs of its quality control. In this study, an off-line hydrophilic interaction×reversed-phase two-dimensional liquid chromatography (HILIC×RP 2D-LC) system coupled with diode array detection (DAD) and quadrupole time-of-flight mass spectrometry (qTOF-MS) was established to comprehensively analyze the chemical constituents of GBE. After optimizing the chromatographic columns and mobile phase of 2D-LC, a Waters XBridge Amide column using acetonitrile/water/formic acid as the mobile phase was selected as the first dimension to fractionate GBE, and the obtained fractions were further separated on an Agilent Zorbax XDB-C18 column with methanol/water/formic acid as the mobile phase. As a result, a total of 125 compounds were detected in GBE. The orthogonality of the 2D-LC system was 69.5%, and the practical peak capacity was 3864 and 2994, respectively, calculated by two different methods. The structures of 104 compounds were tentatively characterized by qTOF-MS analysis, and 21 of them were further confirmed by comparing with reference standards. This established HILIC×RP 2D-LC-qTOF/MS system can greatly improve the separation and characterization of natural products in GBE or other complicated herbal extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of heavy polycyclic aromatic hydrocarbons by non-aqueous reversed phase liquid chromatography: Application and limitation in refining streams.

Science.gov (United States)

Panda, Saroj K; Muller, Hendrik; Al-Qunaysi, Thunayyan A; Koseoglu, Omer R

2018-01-19

The heavy polycyclic aromatic hydrocarbons (HPAHs) cause detrimental effects to hydrocracker operations by deactivating the catalysts and depositing in the downstream of the reactor/ exchangers. Therefore, it is essential to continuously monitor the accumulation of HPAHs in a hydrocracker unit. To accurately measure the concentration of HPAHs, the development of a fast and reliable analytical method is inevitable. In this work, an analytical method based on non-aqueous reversed phase chromatography in combination with high resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was developed. As a first step, five different types of stationary phases were evaluated for the separation of HPAHs in non-aqueous mode and the best suited phase was further used for the fractionation of HPAHs in a fractionator bottom sample obtained from a refinery hydrocracker unit. The eight major fractions or peaks obtained from the separation were further characterized by UV spectroscopy and FT-ICR MS and the compounds in the fractions were tentatively confirmed as benzoperylene, coronene, methylcoronene, naphthenocoronene, benzocoronene, dibenzoperylene, naphthocoronene and ovalene. The developed liquid chromatography method can be easily adapted in a refinery laboratory for the quantitation of HPAHs in hydrocracking products. The method was further tested to check the interference of sulfur aromatics and/or large alkylated aromatic hydrocarbons on the determination of HPAHs in hydrocracking products. Copyright © 2017 Elsevier B.V. All rights reserved.

Reversed-Phase High-Performance Liquid Chromatography for the Quantification and Optimization for Extracting 10 Kinds of Carotenoids in Pepper (Capsicum annuum L.) Leaves.

Science.gov (United States)

Li, Jing; Xie, Jianming; Yu, Jihua; Lv, Jian; Zhang, Junfeng; Wang, Xiaolong; Wang, Cheng; Tang, Chaonan; Zhang, Yingchun; Dawuda, Mohammed Mujitaba; Zhu, Daiqiang; Ma, Guoli

2017-09-27

Carotenoids are considered to be crucial elements in many fields and, furthermore, the significant factor in pepper leaves under low light and chilling temperature. However, little literature focused on the method to determinate and extract the contents of carotenoid compositions in pepper leaves. Therefore, a time-saving and highly sensitive reversed-phase high-performance liquid chromatography method for separation and quantification of 10 carotenoids was developed, and an optimized technological process for carotenoid composition extraction in pepper leaves was established for the first time. Our final method concluded that six xanthophylls eluted after about 9-26 min. In contrast, four carotenes showed higher retention times after nearly 28-40 min, which significantly shortened time and improved efficiency. Meanwhile, we suggested that 8 mL of 20% KOH-methanol solution should be added to perform saponification at 60 °C for 30 min. The ratio of solid-liquid was 1:8, and the ultrasound-assisted extraction time was 40 min.

Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography.

Science.gov (United States)

Roosta, Mostafa; Ghaedi, Mehrorang; Daneshfar, Ali

2014-10-15

A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400μL of distilled water was added and the microextraction was accelerated by 4min sonication. After 8.5min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200mgL(-1). The detection limit of method was 0.2mgL(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n=5) while the recoveries were in the range of 93.9-107.8%. Copyright © 2014. Published by Elsevier Ltd.

Simultaneous liquid chromatography/mass spectrometry determination of both polar and "multiresidue" pesticides in food using parallel hydrophilic interaction/reversed-phase liquid chromatography and a hybrid sample preparation approach.

Science.gov (United States)

Robles-Molina, José; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

2017-09-29

Pesticide testing of foodstuffs is usually accomplished with generic wide-scope multi-residue methods based on liquid chromatography tandem mass spectrometry (LC-MS/MS). However, this approach does not cover some special pesticides, the so called "single-residue method" compounds, that are hardly compatible with standard reversed-phase (RP) separations due to their specific properties. In this article, we propose a comprehensive strategy for the integration of single residue method compounds and standard multiresidue pesticides within a single run. It is based on the use of a parallel LC column assembly with two different LC gradients performing orthogonal hydrophilic interaction chromatography (HILIC) and reversed-phase (RPLC) chromatography within one analytical run. Two sample aliquots were simultaneously injected on each column, using different gradients, being the eluents merged post-column prior to mass spectrometry detection. The approach was tested with 41 multiclass pesticides covering a wide range of physicochemical properties across several orders of log K ow (from -4 to +5.5). With this assembly, distinct separation from the void was attained for all the pesticides studied, keeping similar performance in terms of sensitivity, peak area reproducibility (pesticides) method was evaluated based on solvent extraction with MeOH and acetonitrile followed by dispersive solid-phase extraction, delivering appropriate recoveries for most of the pesticides included in the study within the log K ow in the range from -4 to +5.5. The proposed strategy may be extended to other fields such as sport drug testing or environmental analysis, where the same type of variety of analytes featuring poor retention within a single chromatographic separation occurs. Copyright © 2017 Elsevier B.V. All rights reserved.

A reversed phase high performance liquid chromatography method for the determination of fumonisins B1 and B2 in food and feed using monolithic column and positive confirmation by liquid chromatography/tandem mass spectrometry.

Science.gov (United States)

Khayoon, Wejdan Shakir; Saad, Bahruddin; Salleh, Baharuddin; Ismail, Nor Azliza; Abdul Manaf, Normaliza Hj; Abdul Latiff, Aishah

2010-10-29

The development of a reversed phase high performance liquid chromatography fluorescence method for the determination of the mycotoxins fumonisin B(1) and fumonisin B(2) by using silica-based monolithic column is described. The samples were first extracted using acetonitrile:water (50:50, v/v) and purified by using a C(18) solid phase extraction-based clean-up column. Then, pre-column derivatization for the analyte using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol was carried out. The developed method involved optimization of mobile phase composition using methanol and phosphate buffer, injection volume, temperature and flow rate. The liquid chromatographic separation was performed using a reversed phase Chromolith(®) RP-18e column (100 mm × 4.6 mm) at 30 °C and eluted with a mobile phase of a mixture of methanol and phosphate buffer pH 3.35 (78:22, v/v) at a flow rate of 1.0 mL min(-1). The fumonisins separation was achieved in about 4 min, compared to approximately 20 min by using a C(18) particle-packed column. The fluorescence excitation and emission were at 335 nm and 440 nm, respectively. The limits of detections were 0.01-0.04 μg g(-1) fumonisin B(1) and fumonisin B(2), respectively. Good recoveries were found for spiked samples (0.1, 0.5, 1.5 μg g(-1) fumonisins B(1) and B(2)), ranging from 84.0 to 106.0% for fumonisin B(1) and from 81.0 to 103.0% for fumonisin B(2). Fifty-three samples were analyzed including 39 food and feeds and 14 inoculated corn and rice. Results show that 12.8% of the food and feed samples were contaminated with fumonisin B(1) (range, 0.01-0.51 μg g(-1)) and fumonisin B(2) (0.05 μg g(-1)). The total fumonisins in these samples however, do not exceed the legal limits established by the European Union of 0.8 μg g(-1). Of the 14 inoculated samples, 57.1% contained fumonisin B(1) (0.16-41.0 μg g(-1)) and fumonisin B(2) (range, 0.22-50.0 μg g(-1)). Positive confirmation of selected samples was carried out using

Column Liquid Chromatography.

Science.gov (United States)

Majors, Ronald E.; And Others

1984-01-01

Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

Thermodynamics of the sorption of water-soluble vitamins in reverse-phase high performance liquid chromatography

Science.gov (United States)

Chirkin, V. A.; Karpov, S. I.; Selemenev, V. F.

2012-12-01

The thermodynamics of the sorption of certain water-soluble vitamins on a C18 reverse phase from water-acetonitrile solutions of different compositions is studied. The thermodynamic characteristics of the investigated chromatographic systems are calculated. The dependences of standard molar enthalpy and changes in entropy when the sorbate transfers from the bulk solution to the surface layer on the concentration of the organic component in the mobile phase are analyzed. The boundaries for applying the main retention models describing the sorption of the investigated compounds are discussed.

Rapid purification of radioiodinated peptides with Sep-Pak reversed phase cartridges and HPLC

International Nuclear Information System (INIS)

Miller, J.J.; Schultz, G.S.; Levy, R.S.

1984-01-01

A simple, rapid method is described for the purification of radioiodinated peptides for use in radioimmuno- and in radioreceptor assays. Iodinated reaction mixtures are applied directly onto Sep-Pak disposable, reversed phase cartridges equilibrated with phosphate buffer. Unreacted 125-iodide and other non-peptide reaction components are eluted with buffer. The peptide fraction is then eluted with 70% buffer:30% acetonitrile. The peptide fraction is further purified by reversed phase high pressure liquid chromatography to separate the native peptide and the mono- and diiodo-derivatives. In this study the method is used to prepare 125-iodide-labeled monoiodo-leucine enkephalin and monoiodo-angiotensin II, which are free of the parent peptides and diiodo-derivatives and are of maximum obtainable specific radioactivity. The usefulness of these labeled peptides in radioimmuno- and radioreceptor assays is demonstrated by their binding to specific antibodies and receptors, respectively. (author)

A review of solid-fluid selection options for optical-based measurements in single-phase liquid, two-phase liquid-liquid and multiphase solid-liquid flows

Science.gov (United States)

Wright, Stuart F.; Zadrazil, Ivan; Markides, Christos N.

2017-09-01

Experimental techniques based on optical measurement principles have experienced significant growth in recent decades. They are able to provide detailed information with high-spatiotemporal resolution on important scalar (e.g., temperature, concentration, and phase) and vector (e.g., velocity) fields in single-phase or multiphase flows, as well as interfacial characteristics in the latter, which has been instrumental to step-changes in our fundamental understanding of these flows, and the development and validation of advanced models with ever-improving predictive accuracy and reliability. Relevant techniques rely upon well-established optical methods such as direct photography, laser-induced fluorescence, laser Doppler velocimetry/phase Doppler anemometry, particle image/tracking velocimetry, and variants thereof. The accuracy of the resulting data depends on numerous factors including, importantly, the refractive indices of the solids and liquids used. The best results are obtained when the observational materials have closely matched refractive indices, including test-section walls, liquid phases, and any suspended particles. This paper reviews solid-liquid and solid-liquid-liquid refractive-index-matched systems employed in different fields, e.g., multiphase flows, turbomachinery, bio-fluid flows, with an emphasis on liquid-liquid systems. The refractive indices of various aqueous and organic phases found in the literature span the range 1.330-1.620 and 1.251-1.637, respectively, allowing the identification of appropriate combinations to match selected transparent or translucent plastics/polymers, glasses, or custom materials in single-phase liquid or multiphase liquid-liquid flow systems. In addition, the refractive indices of fluids can be further tuned with the use of additives, which also allows for the matching of important flow similarity parameters such as density and viscosity.

Modeling of liquid phases

CERN Document Server

Soustelle, Michel

2015-01-01

This book is part of a set of books which offers advanced students successive characterization tool phases, the study of all types of phase (liquid, gas and solid, pure or multi-component), process engineering, chemical and electrochemical equilibria, and the properties of surfaces and phases of small sizes. Macroscopic and microscopic models are in turn covered with a constant correlation between the two scales. Particular attention has been given to the rigor of mathematical developments. This second volume in the set is devoted to the study of liquid phases.

Towards a physical interpretation of third phase formation in liquid-liquid extraction. Application to the Diamex process for the treatment of high radioactive nuclear wastes

International Nuclear Information System (INIS)

Verdier Erlinger, C.

1998-07-01

Using SAXS, conductivity and phase behaviour determination we show that concentrated solutions of extractants are organised in reverse oligomeric aggregates which have many features in common with reverse micelles. The aggregation numbers of these reverse globular aggregates as well as their interaction potential are determined experimentally. The sticky sphere interaction is responsible for the unmixing of the oil phase when in equilibrium with excess oil. Prediction of conductivity as well as formation condition for the third phase is possible using standard liquid theory applied to the reverse micelles, The attractive interaction, modelled with the sticky sphere model proposed by Baxter, is the balance of steric stabilisation introduced by the hydrophobic tails of the extracting molecule and the Van der Waals forces between the highly polarizable water core of the reverse micelles. Attraction in the oil phase, equilibrated with water, is determined versus temperature, extractant molecule concentration, number of carbon atoms of aliphatic solvents, as well as proton and Neodymium cation concentration.-It is shown that van der Waals interactions with a Hamaker constant of 2.5 kT explains the behaviour of DMDBTDMA in dodecane. (author)

Towards a physical interpretation of third phase formation in liquid-liquid extraction. Application to the Diamex process for the treatment of high radioactive nuclear wastes

International Nuclear Information System (INIS)

Verdier-Erlinger, C.

1998-01-01

Using SAXS, conductivity and phase behaviour determination we show that concentrated solutions of extractants are organised in reverse oligomeric aggregates which have many features in common with reverse micelles. The aggregation numbers of these reverse globular aggregates as well as their interaction potential are determined experimentally. The sticky sphere interaction is responsible for the de-mixing on the oil phase when in equilibrium with excess oil. Prediction of conductivity as well as formation condition for the third phase is possible using standard liquid theory applied to the reverse micelles. The attractive interaction, modeled with the sticky sphere model proposed by Baxter, is the balance of steric stabilisation introduced by the hydrophobic tails of the extracting molecule and the Van der Waals forces between the highly polarizable water core of the reverse molecule concentration, number of carbon atoms of aliphatic solvents, as well as proton and Neodymium cation concentration. It is shown that van der Waals interactions with a Hamaker constant of 2.5 kT explains the behaviour of DMDBTDMA in dodecane. (author)

Iron Fibers Arrays Prepared by Electrodepositing in Reverse Liquid Crystalline

Institute of Scientific and Technical Information of China (English)

ZHAO Suling; LIN Dong; GUAN Jianguo; ZHANG Lianmeng

2006-01-01

Ordered iron fiber arrays were electrodeposited on the surface of zinc foils using "FeSO4 solution-sodium caprylate-Decanol" 3-component reverse hexagonal liquid crystal as soft templates. The structure of the soft templates and the synthesized iron fibers were characterized by polarizing microscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray microanalysis etc. The experimental results show that the synthesized iron fibers with α crystal phase grew up in the form of fiber clusters of about 200 nm along the direction perpendicular to the cathode surface. Each cluster was composed of several tens of fibers. The fibers had almost the same length of more than 10 μm with a diameter of about 50 nm.

Stress degradation studies of Telmisartan and Metoprolol extended release tablets by a validated stability indicating reverse phase-high performance liquid chromatography method

Directory of Open Access Journals (Sweden)

Kabeer Ahmed Shaikh

2014-01-01

Full Text Available Background and Aim: A sensitive reverse phase high-performance liquid chromatographic method has been developed for the simultaneous determination of Telimisartan and Metoprolol in tablet dosage form. Materials and Method: The chromatographic separation was achieved on Inertsil ODS 3V, 150 x 4.6 mm, 5μ analytical column. Mobile phase consisting of mobile phase A- 0.05M sodium dihydrogen phosphate buffer pH 3.0 and mobile phase B-Acetonitrile, with gradient program time in min /Mobile phase B% 0/22, 4/45, 6/45,18/22, 20/22. Detector was set at 222nm. Results and Conclusion: The described method shows excellent linearity over a range of 80-2 μg mL−1 for Telmisartan and 100-4 μg mL−1 for Metoprolol. The correlation coefficient for Telmisartan is 0.9998 and Metoprolol is 0.9999. The proposed method was found to be suitable for determination of Telmisartan and Metoprolol in tablet dosage form. Forced degradation of the drug product was conducted in accordance with the ICH guideline. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation was used to assess the stability indicating power of the method. The drug product was found to be stable in acid, oxidation, thermal and photolytic stress condition and found degradation in base hydrolysis stress condition.

Surface passivation of liquid phase epitaxial GaAs

International Nuclear Information System (INIS)

Alexiev, D.; Butcher, K.S.A.; Mo, L.; Edmondson, M.

1995-10-01

Passivation of the liquid phase epitaxial GaAs surface was attempted using aqueous P 2 S 5 -NH 4 OH, (NH 4 ) 2 S x and plasma nitrogenation and hydrogenation. Results indicate that plasma nitrogenation with pretreatment of plasma hydrogenation produced consistent reduction in reverse leakage current at room temperature for all p and n type Schottky diodes. Some diodes showed an order of magnitude improvement in current density. (NH 4 ) 2 S x passivation also results in improved I-V characteristics, though the long term stability of this passivation is questionable. 26 refs., 6 figs

[Separation of p-aminobenzenearsonic acid and its oxide by ion-pair reversed-phase high performance liquid chromatography].

Science.gov (United States)

Kang, J; Ma, X; Meng, L; Ma, D

1999-05-01

To study the separation of p-aminobenzenearsonic acid (PABAA) and its oxide, p-aminophenylarsine oxide (PAPAO), both the absorption spectra were scanned at the wavelengths from 200 nm to 380 nm. PABAA had absorption maximum at 254 nm and PAPAO 258 nm. The effects of salt concentration, column temperature, methanol and ion-pair agent concentrations on the capacity factor were investigated. Compounds of high polarity showed almost no retention on reversed-phase column; as the volume fraction of the methanol decreased from 90% to 10%, the retention time of PABAA gradually increased with broad peak, and partially eluted when methanol volume fraction being below 20%. With temperature rising, the retention time of PABAA was decreased. But PABAA capacity factor can be increased by selecting an appropriate salt concentration for the mobile phase. The cetyltrimethyl and tetrabutyl ammonium ions were separately added as ion-pair agents to the mobile phase containing methanol in phosphate buffer of 10 mmol/L, the changes of retention time were observed. The mechanism of retention based on reversed phase ion-pair model is proposed. Besides, the retention behaviour is also influenced by size exclusion in stationary phase as well as polar interactions with residual silanol group on the silica surface.

Two-step ion-exchange chromatographic purification combined with reversed-phase chromatography to isolate C-peptide for mass spectrometric analysis.

Science.gov (United States)

Kabytaev, Kuanysh; Durairaj, Anita; Shin, Dmitriy; Rohlfing, Curt L; Connolly, Shawn; Little, Randie R; Stoyanov, Alexander V

2016-02-01

A liquid chromatography with mass spectrometry on-line platform that includes the orthogonal techniques of ion exchange and reversed phase chromatography is applied for C-peptide analysis. Additional improvement is achieved by the subsequent application of cation- and anion-exchange purification steps that allow for isolating components that have their isoelectric points in a narrow pH range before final reversed-phase mass spectrometry analysis. The utility of this approach for isolating fractions in the desired "pI window" for profiling complex mixtures is discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Putative Liquid-Liquid Transition is a Liquid-Solid Transition in Atomistic Models of Water

Science.gov (United States)

Chandler, David; Limmer, David

2013-03-01

Our detailed and controlled studies of free energy surfaces for models of water find no evidence for reversible polyamorphism, and a general theoretical analysis of the phase behavior of cold water in nano pores shows that measured behaviors of these systems reflect surface modulation and dynamics of ice, not a liquid-liquid critical point. A few workers reach different conclusions, reporting evidence of a liquid-liquid critical point in computer simulations of supercooled water. In some cases, it appears that these contrary results are based upon simulation algorithms that are inconsistent with principles of statistical mechanics, such as using barostats that do not reproduce the correct distribution of volume fluctuations. In other cases, the results appear to be associated with difficulty equilibrating the supercooled material and mistaking metastability for coarsening of the ordered ice phase. In this case, sufficient information is available for us to reproduce the contrary results and to establish that they are artifacts of finite time sampling. This finding leads us to the conclusion that two distinct, reversible liquid phases do not exist in models of supercooled water.

Determination of vitamin E acid succinate in biodegradable microspheres by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Martínez Sancho, C; Herrero Vanrell, R; Negro, S

2004-01-01

A simple, rapid, and reproducible reversed-phase high-performance liquid chromatographic (HPLC) method is applied to the routine assay of vitamin E acid succinate in biodegradable microspheres. Vitamin E acid-succinate-containing poly-(D,L-lactic-co-glycolic acid) microspheres are prepared by the solvent evaporation method. The starting drug-polymer ratio is 1:10 (w/w) and the total amount of drug and polymer processed is always 440 mg. The content of vitamin E acid succinate in the microspheres is evaluated by HPLC. Chromatography is carried out isocratically at 25 degrees C +/- 0.5 degrees C on an Extrasil ODS-2 column with a mobile phase composed of methanol-water (97:3, v/v) (pH 5.6) at a flow rate of 2 mL/min and UV detection at 284 nm. Parameters such as linearity, limits of quantitation (LOQ) and detection (LOD), precision, accuracy, recovery, specificity, and ruggedness are studied as reported in the International Conference on Harmonization guidelines. The stability of vitamin E acid succinate is also studied with satisfactory results after 48 h at 25 degrees C. The method is selective and linear for drug concentrations in the range 15-210 micro g/mL. The LOQ and LOD are 15 and 3 micro g/mL, respectively. The results for accuracy studies are good. Values for coefficient of variation for intra- and interassay are 2.08% and 2.32%, respectively. The mean percentage of vitamin E acid succinate in the recovery studies is 99.52% +/- 0.81%. The mean loading efficiency for microspheres is 96.53% +/- 1.31%.

Development and validation of reverse phase high performance liquid chromatography for citral analysis from essential oils.

Science.gov (United States)

Gaonkar, Roopa; Yallappa, S; Dhananjaya, B L; Hegde, Gurumurthy

2016-11-15

Citral is a widely used monoterpene aldehyde in aromatherapy, food and pesticide industries. A new validated reverse phase high performance liquid chromatography (RP - HPLC) procedure for the detection and quantification of cis-trans isomers of citral was developed. The RP-HPLC analysis was carried out using Enable C - 18G column (250×4.6mm, 5μ), with acetonitrile and water (70: 30) mobile phase in isocratic mode at 1mL/min flow. A photodiode array (PDA) detector was set at 233nm for the detection of citral. The method showed linearity, selectivity and accuracy for citral in the range of 3-100μg/mL. In order to compare the new RP-HPLC method with the available methods, one of the commercially available essential oil from Cymbopogon flexuosus was analyzed using new RP-HPLC method and the same was analyzed using GC-MS for the comparison of the method for the detection of citral. The GC-MS analysis was done using mass selective detector (MSD) showed citral content to be of 72.76%; wherein the new method showed to contain that same at 74.98%. To prove the application of the new method, essential oils were extracted from lemongrass, lemon leaves and mosambi peels by steam distillation. The citral content present in the essential and also in the condensate was analyzed. The method was found to be suitable for the analysis of citral in essential oils and water based citral formulations with a very good resolution of its components geranial and neral. Copyright © 2016 Elsevier B.V. All rights reserved.

Histone fractionation by high-performance liquid chromatography on cyanoalkylsilane (CN) reverse-phase columns

International Nuclear Information System (INIS)

Gurley, L.R.; Prentice, D.A.; Valdez, J.G.; Spall, W.D.

1983-01-01

Previous work described conditions for the rapid fractionation of histones by high-performance liquid chromatography (HPLC) using a reverse-phase μBondapak C 18 column. That procedure resolved the major classes of histones with one exception: the more hydrophobic H2A variant, (MHP)H2A, was not resolved from the H4 histone class. This report extends that work describing experiments using a μBondapak CN column which better resolves the classes of histones from each other including the resolution of (MHP)H2A from the H4. In addition, the less hydrophobic H2A variant, (LHP)H2A, is partially resolved from the (MHP)H2A, and the less hydrophobic H3 variant, (LHP)H3, is resolved from the more hydrophobic H3 variant, (MHP)H3. Lower trifluoroacetic acid (TFA) concentrations (0.1%) in the eluting water/acetonitrile solvent were used with the CN column than were used with the C 18 column which increased the sensitivity of histone detection by ultraviolet absorption at 206 nm. Greater than 95% of the total [ 3 H]lysine-labeled protein applied to the CN column was eluted from the column. Contaminating nonhistone proteins were found to chromatograph in the region of histone elution. These were greatly reduced by isolating nuclei prior to histone preparation. The fractionation of the histones appears to be based on the hydrophobic properties of the proteins. The histone fractions (identified by their electrophoretic mobilities) were eluted from the CN column in the following order: H1, H2B, (LHP)H2A, (MHP)H2A, H4, (LHP)H3, and (MHP)H3. Phosphorylated and acetylated histone species were not resolved from their unmodified parental species

Simultaneous determination of seven synthetic colorants in wine by dispersive micro-solid-phase extraction coupled with reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Zhang, Yun; Zhou, Hua; Wang, Yougang; Wu, Xianglun; Zhao, Yonggang

2015-02-01

A novel and effective dispersive micro-solid-phase extraction (d-µ-SPE) using ethanediamine-functionalized magnetic Fe3O4 polymer (EDA-MP) as an efficient adsorbent in wine sample was developed. Based on this, a simple and time-saving analytical method for the simultaneous determination of seven synthetic colorants (i.e., tartrazine, amaranth, carmine, sunset yellow, allura red, brilliant blue and erythrosine) in wine by reversed-phase high-performance liquid chromatography with an ultraviolet detector was established. The experimental parameters, including the chromatographic retention behavior of studied synthetic colorants, the effect of the usage amount of cross-linking monomer, the effect of the usage amount of EDA-MP on the recovery and the recyclability of the adsorbents, were studied in detail. The results showed that the EDA-MP could be reused efficiently at least six times. Under optimized conditions, the recoveries for all analytes were in the range of 88.6-105.2%, with the intraday relative standard deviations (RSDs) ranging from 2.1 to 8.2% and the interday RSDs ranging from 3.4 to 8.7%, and all the analytes had good linearities in the tested ranges with correlation coefficients (r(2)) >0.9995. The limits of quantification for seven synthetic colorants were between 0.12 and 0.45 mg L(-1). The developed method was successfully applied to wine samples, and it was confirmed that the EDA-MP particles were highly effective d-µ-SPE materials. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Recent development of ionic liquid stationary phases for liquid chromatography.

Science.gov (United States)

Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

2015-11-13

Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

Modelling of the effect of solute structure and mobile phase pH and composition on the retention of phenoxy acid herbicides in reversed-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Aschi, Massimiliano; D'Archivio, Angelo Antonio; Mazzeo, Pietro; Pierabella, Mirko; Ruggieri, Fabrizio

2008-01-01

A feed-forward artificial neural network (ANN) learned by error back-propagation is used to generate a retention predictive model for phenoxy acid herbicides in isocratic reversed-phase high-performance liquid chromatography. The investigated solutes (18 compounds), apart from the most common herbicides of this class, include some derivatives of benzoic acid and phenylacetic acid structurally related to phenoxy acids, as a whole covering a pK a range between 2.3 and 4.3. A mixed model in terms of both solute descriptors and eluent attributes is built with the aim of predicting retention in water-acetonitrile mobile phases within a large range of composition (acetonitrile from 30% to 70%, v/v) and acidity (pH of water before mixing with acetonitrile ranging between 2 and 5). The set of input variables consists of solute pK a and quantum chemical molecular descriptors of both the neutral and dissociated form, %v/v of acetonitrile in the mobile phase and pH of aqueous phase before mixing with acetonitrile. After elimination of redundant variables, a nine-dimensional model is identified and its prediction ability is evaluated by external validation based on three solutes not involved in model generation and by cross-validation. A multilinear counterpart in terms of the same descriptors is seen to provide a noticeably poorer retention prediction

Modelling of the effect of solute structure and mobile phase pH and composition on the retention of phenoxy acid herbicides in reversed-phase high-performance liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Aschi, Massimiliano [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); D' Archivio, Angelo Antonio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)], E-mail: darchivi@univaq.it; Mazzeo, Pietro; Pierabella, Mirko; Ruggieri, Fabrizio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)

2008-06-02

A feed-forward artificial neural network (ANN) learned by error back-propagation is used to generate a retention predictive model for phenoxy acid herbicides in isocratic reversed-phase high-performance liquid chromatography. The investigated solutes (18 compounds), apart from the most common herbicides of this class, include some derivatives of benzoic acid and phenylacetic acid structurally related to phenoxy acids, as a whole covering a pK{sub a} range between 2.3 and 4.3. A mixed model in terms of both solute descriptors and eluent attributes is built with the aim of predicting retention in water-acetonitrile mobile phases within a large range of composition (acetonitrile from 30% to 70%, v/v) and acidity (pH of water before mixing with acetonitrile ranging between 2 and 5). The set of input variables consists of solute pK{sub a} and quantum chemical molecular descriptors of both the neutral and dissociated form, %v/v of acetonitrile in the mobile phase and pH of aqueous phase before mixing with acetonitrile. After elimination of redundant variables, a nine-dimensional model is identified and its prediction ability is evaluated by external validation based on three solutes not involved in model generation and by cross-validation. A multilinear counterpart in terms of the same descriptors is seen to provide a noticeably poorer retention prediction.

Evaluating the Liquid Liquid Phase Transition Hypothesis of Supercoooled Water

Science.gov (United States)

Limmer, David; Chandler, David

2011-03-01

To explain the anomalous behavior of supercooled water it has been conjectured that buried within an experimentally inaccessible region of liquid water's phase diagram there exists a second critical point, which is the terminus of a first order transition line between two distinct liquid phases. The so-called liquid-liquid phase transition (LLPT) has since generated much study, though to date there is no consensus on its existence. In this talk, we will discuss our efforts to systematically study the metastable phase diagram of supercooled water through computer simulation. By employing importance-sampling techniques, we have calculated free energies as a function of the density and long-range order to determine unambiguously if two distinct liquid phases exist. We will argue that, contrary to the LLPT hypothesis, the observed phenomenology can be understood as a consequence of the limit of stability of the liquid far away from coexistence. Our results suggest that homogeneous nucleation is the cause of the increased fluctuations present upon supercooling. Further we will show how this understanding can be extended to explain experimental observations of hysteresis in confined supercooled water systems.

Characterisation of UV-cured acrylate networks by means of hydrolysis followed by aqueous size-exclusion combined with reversed-phase chromatography

NARCIS (Netherlands)

Peters, R.; Litvinov, V. M.; Steeman, P.; Dias, A. A.; Mengerink, Y.; van Benthem, R.; de Koster, C. G.; van der Wal, S. J.; Schoenmakers, P.

2007-01-01

UV-cured networks prepared from mixtures of di-functional (polyethylene-glycol di-acrylate) and mono-functional (2-ethylhexyl acrylate) acrylates were analysed after hydrolysis, by aqueous size-exclusion chromatography coupled to on-line reversed-phase liquid-chromatography. The mean network density

[High-performance liquid-liquid chromatography in beverage analysis].

Science.gov (United States)

Bricout, J; Koziet, Y; de Carpentrie, B

1978-01-01

Liquid liquid chromatography was performed with columns packed with stationary phases chemically bonded to silica microparticules. These columns show a high efficiency and are used very easily. Flavouring compounds like aromatic aldehydes which have a low volatility were analyzed in brandy using a polar phase alkylnitrile. Sapid substances like amarogentin in Gentiana lutea or glyryrrhizin in Glycyrrhiza glabra were determined by reversed phase chromatography. Finally ionizable substances like synthetic dyes can be analyzed by paired ion chromatography witha non polar stationary phase.

Estimation of Rabeprazole Sodium and Itopride Hydrochloride in Tablet Dosage Form Using Reverse Phase High Performance Liquid Chromatography

Directory of Open Access Journals (Sweden)

Shaik Harum Rasheed

2011-01-01

Full Text Available A reversed phase high performance liquid chromatography (RP-HPLC method was developed, validated and used for the quantitative determination of rabeprazole sodium (RP and itopride hydrochloride (IH, from its tablet dosage form. Chromatographic separation was performed on a Phenomenex C18 column (250 mm × 4.6 mm, 5 μm, with a mobile phase comprising of a mixture of 50 mM ammonium acetate buffer and methanol (20:80v/v, pH 4.5 adjusted with acetic acid, at a flow rate of 1.3 mL/min with detection at 286 nm. Separation was completed in less than 10 min. As per International Conference on Harmonization (ICH guidelines the method was validated for linearity, accuracy, precision, limit of quantitation and limit of detection. Linearity of RP was found to be in the range of 37.5-375 μg/mL and IH was found to be in the range of 5-50 μg/mL. The correlation coefficients were 0.9997 and 0.9995 for RB and IH respectively. The accuracy of the developed method was found to be 98.6-100.7 for RP and 99.42 -100.81 for IH. The experiment shows the developed method is free from interference of excipients. It indicates the developed RP-HPLC method is simple, linear, precise and accurate and it can be conveniently adopted for the routine quality control analysis of the tablet dosage form.

Copolymer-grafted silica phase from a cation-anion monomer pair for enhanced separation in reversed-phase liquid chromatography.

Science.gov (United States)

Mallik, Abul K; Qiu, Hongdeng; Takafuji, Makoto; Ihara, Hirotaka

2014-05-01

This work reports a new imidazolium and L-alanine derived copolymer-grafted silica stationary phase for ready separation of complex isomers using high-performance liquid chromatography (HPLC). For this purpose, 1-allyl-3-octadecylimidazolium bromide ([AyImC18]Br) and N-acryloyl-L-alanine sodium salt ([AAL]Na) ionic liquids (IL) monomers were synthesized. Subsequently, the bromide counteranion was exchanged with the 2-(acrylamido)propanoate organic counteranion by reacting the [AyImC18]Br with excess [AAL]Na in water. The obtained IL cation-anion monomer pair was then copolymerized on mercaptopropyl-modified silica (Sil-MPS) via a surface-initiated radical chain-transfer reaction. The selective retention behaviors of polycyclic aromatic hydrocarbons (PAHs), including some positional isomers, steroids, and nucleobases were investigated using the newly obtained Sil-poly(ImC18-AAL), and octadecyl silylated silica (ODS) was used as the reference column. Interesting results were obtained for the separation of PAHs, steroids, and nucleobases with the new organic phase. The results showed that the Sil-poly(ImC18-AAL) presented multiple noncovalent interactions, including hydrophobic, π-π, carbonyl-π, and ion-dipole interactions for the separation of PAHs and dipolar compounds. Only pure water was sufficient as the mobile phase for the separation of the nucleobases. Ten nucleosides and bases were separated, using only water as the mobile phase, within a very short time using the Sil-poly(ImC18-AAL), which is otherwise difficult to achieve using conventional hydrophobic columns such as ODS. The combination of electrostatic and hydrophobic interactions are important for the effective separation of such basic compounds without the use of any organic additive as the eluent on the Sil-poly(ImC18-AAL) column.

Liquid radwaste treatment by microfiltration, ultrafiltration and reverse osmosis

International Nuclear Information System (INIS)

Dulama, M.; Deneanu, N.; Popescu, I.V.

2001-01-01

Radioactive liquid waste processing is an integral part of any facility involved in nuclear power generation, radioisotope production, research and development, decontamination or other aspects of nuclear energy. The aqueous liquid radwastes from the decontamination center are currently treated by the membrane plant. Generally, the liquid waste streams are effectively volume-reduced by a combination of continuous crossflow microfiltration (MF), spiral wound reverse osmosis (SWRO) and tubular reverse osmosis membrane technologies. Backwash chemical cleaning wastes from the membrane plant are further volume-reduced by evaporation. The concentrate from the membrane plant is ultimately immobilized with bitumen. We performed experiments using two simulated waste solution; secondary waste from the decontamination process with POD (Permanganate Oxidation Decontamination) solution and secondary waste from decontamination with CAN-DECON solution. The experimental tests have been done with cellulose acetate (CA) membrane and polysulfonate (PSF) membrane manufactured at Research Center for Macromolecular Materials and Membranes Bucharest and with Millipore membrane type VS 0.025 μm. A schematic of the laboratory-scale test facility is presented

Development and Validation of a Reversed-Phase Liquid Chromatography Method for the Simultaneous Determination of Indole-3-Acetic Acid, Indole-3-Pyruvic Acid, and Abscisic Acid in Barley (Hordeum vulgare L.).

Science.gov (United States)

Nakurte, Ilva; Keisa, Anete; Rostoks, Nils

2012-01-01

A simple, sensitive, precise, and specific reverse HPLC method was developed and validated for the determination of plant hormones in barley (Hordeum vulgare L.). The method includes extraction in aqueous organic solvent followed by solid-phase extraction, sample evaporation, and reversed-phase HPLC analysis in a general purpose UV-visible (abscisic acid (ABA)) and fluorescence detection (indole-3-acetic acid (IAA) and indole-3-pyruvic acid (IPA)), high-performance liquid chromatography system. The separation was carried out on Zorbax Eclipse XDB C8 column (150  ×  4.6  mm I.D) with a mobile phase composed of methanol and 1% acetic acid (60 : 40 v/v) in isocratic mode at a flow rate of 1 ml min(-1). The detection was monitored at 270 nm (ABA) and at 282 nm (Ex) and 360 nm (Em) (IAA, IPA). The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification, and robustness. The determined validation parameters are in the commonly acceptable ranges for that kind of analysis.

[Influences of ion-suppressors on retention behaviors of nine food additives in reversed-phase high performance liquid chromatographic separation].

Science.gov (United States)

Zhao, Yonggang; Chen, Xiaohong; Li, Xiaoping; Yao, Shanshan; Jin, Micong

2011-10-01

The influences of ion-suppressors on retention behaviors of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in reversed-phase high performance liquid chromatographic (RP-HPLC) separation were investigated. The organic modification effects of acids, i. e. , trifluoroacetic acid (TFA) and buffer salts, i. e. , TFA-ammonium acetate (AmAc) were studied emphatically. The relationships between retention factors of solutes and volume percentages of ion-suppressors in the mobile phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, separately. The separation of nine food additives was completed by a gradient elution with acetonitrile-TFA (0.01%, v/v)-AmAc (2. 5 mmol/L) aqueous solution as the mobile phases. An RP-HPLC method was established for the simultaneous determination of nine food additives in red wine. In the range of 10. 0 - 100. 0 mg/L, nine food additives showed good linearity with the correlation coefficients ( r2 ) larger than 0. 999 1. The limits of detection (LODs) were in the range of 0. 33 - 2. 36 mg/L and the limits of quantification (LOQs) were in the range of 1. 11 - 7. 80 mg/L. The spiked recoveries were between 87. 61% and 108. 4% with the relative standard deviations (RSDs) of 2. 2% -9. 4%. These results are of referential significance for the rapid establishment and accu- rate optimization of RP-HPLC separation for the simultaneous determination of food additives in other foods.

How to separate ionic liquids: Use of Hydrophilic Interaction Liquid Chromatography and mixed mode phases

International Nuclear Information System (INIS)

Lamouroux, C.

2011-01-01

This chromatographic study deals with the development of a convenient and versatile method to separate Room Temperature Ionic Liquids. Different modes of chromatography were studied. The study attempts to answer the following question: 'what were the most important interactions for the separation of ionic liquids?'. The results show that the essential interactions to assure a good retention of RTILs are the ionic ones and that hydrophobic interactions play a role in the selectivity of the separation. The separation of five imidazolium salt with a traditional dial columns in Hydrophilic Interaction Chromatography (HILIC) was demonstrated. It shows that neutral diol grafted column allows an important retention that we assume is due to the capability of diol to develop a thick layer of water. Furthermore, stationary phase based on mixed interaction associating ion exchange and hydrophobic properties were studied. Firstly, it will be argued that it is possible to separate RTILs with a convenient retention and resolution according to a reverse phase elution with the Primesep columns made of a brush type long alkyl chain with an embedded negatively charged functional group. Secondly, a successful separation of RTILs in HILIC mode with a mixed phase column containing a cationic exchanger and a hydrophobic octyl chain length will be demonstrated. (author)

Cloud-point extraction and reversed-phase high-performance liquid chromatography for the determination of synthetic phenolic antioxidants in edible oils.

Science.gov (United States)

Chen, Miao; Xia, Qinghai; Liu, Mousheng; Yang, Yaling

2011-01-01

A cloud-point extraction (CPE) method using Triton X-114 (TX-114) nonionic surfactant was developed for the extraction and preconcentration of propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) from edible oils. The optimum conditions of CPE were 2.5% (v/v) TX-114, 0.5% (w/v) NaCl and 40 min equilibration time at 50 °C. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid chromatography with ultraviolet detection at 280 nm, using a gradient mobile phase consisting of methanol and 1.5% (v/v) acetic acid. Under the studied conditions, 4 synthetic phenolic antioxidants (SPAs) were successfully separated within 24 min. The limits of detection (LOD) were 1.9 ng mL(-1) for PG, 11 ng mL(-1) for TBHQ, 2.3 ng mL(-1) for BHA, and 5.9 ng mL(-1) for BHT. Recoveries of the SPAs spiked into edible oil were in the range 81% to 88%. The CPE method was shown to be potentially useful for the preconcentration of the target analytes, with a preconcentration factor of 14. Moreover, the method is simple, has high sensitivity, consumes much less solvent than traditional methods, and is environment-friendly. Practical Application: The method established in this article uses less organic solvent to extract SPAs from edible oils; it is simple, highly sensitive and results in no pollution to the environment.

The putative liquid-liquid transition is a liquid-solid transition in atomistic models of water. II

Science.gov (United States)

Limmer, David T.; Chandler, David

2013-06-01

This paper extends our earlier studies of free energy functions of density and crystalline order parameters for models of supercooled water, which allows us to examine the possibility of two distinct metastable liquid phases [D. T. Limmer and D. Chandler, J. Chem. Phys. 135, 134503 (2011), 10.1063/1.3643333 and preprint arXiv:1107.0337 (2011)]. Low-temperature reversible free energy surfaces of several different atomistic models are computed: mW water, TIP4P/2005 water, Stillinger-Weber silicon, and ST2 water, the last of these comparing three different treatments of long-ranged forces. In each case, we show that there is one stable or metastable liquid phase, and there is an ice-like crystal phase. The time scales for crystallization in these systems far exceed those of structural relaxation in the supercooled metastable liquid. We show how this wide separation in time scales produces an illusion of a low-temperature liquid-liquid transition. The phenomenon suggesting metastability of two distinct liquid phases is actually coarsening of the ordered ice-like phase, which we elucidate using both analytical theory and computer simulation. For the latter, we describe robust methods for computing reversible free energy surfaces, and we consider effects of electrostatic boundary conditions. We show that sensible alterations of models and boundary conditions produce no qualitative changes in low-temperature phase behaviors of these systems, only marginal changes in equations of state. On the other hand, we show that altering sampling time scales can produce large and qualitative non-equilibrium effects. Recent reports of evidence of a liquid-liquid critical point in computer simulations of supercooled water are considered in this light.

The putative liquid-liquid transition is a liquid-solid transition in atomistic models of water. II

International Nuclear Information System (INIS)

Limmer, David T.; Chandler, David

2013-01-01

This paper extends our earlier studies of free energy functions of density and crystalline order parameters for models of supercooled water, which allows us to examine the possibility of two distinct metastable liquid phases [D. T. Limmer and D. Chandler, J. Chem. Phys.135, 134503 (2011) and preprint http://arxiv.org/abs/arXiv:1107.0337 (2011)]. Low-temperature reversible free energy surfaces of several different atomistic models are computed: mW water, TIP4P/2005 water, Stillinger-Weber silicon, and ST2 water, the last of these comparing three different treatments of long-ranged forces. In each case, we show that there is one stable or metastable liquid phase, and there is an ice-like crystal phase. The time scales for crystallization in these systems far exceed those of structural relaxation in the supercooled metastable liquid. We show how this wide separation in time scales produces an illusion of a low-temperature liquid-liquid transition. The phenomenon suggesting metastability of two distinct liquid phases is actually coarsening of the ordered ice-like phase, which we elucidate using both analytical theory and computer simulation. For the latter, we describe robust methods for computing reversible free energy surfaces, and we consider effects of electrostatic boundary conditions. We show that sensible alterations of models and boundary conditions produce no qualitative changes in low-temperature phase behaviors of these systems, only marginal changes in equations of state. On the other hand, we show that altering sampling time scales can produce large and qualitative non-equilibrium effects. Recent reports of evidence of a liquid-liquid critical point in computer simulations of supercooled water are considered in this light

The putative liquid-liquid transition is a liquid-solid transition in atomistic models of water. II

Energy Technology Data Exchange (ETDEWEB)

Limmer, David T.; Chandler, David, E-mail: chandler@berkeley.edu [Department of Chemistry, University of California, Berkeley, California 94720 (United States)

2013-06-07

This paper extends our earlier studies of free energy functions of density and crystalline order parameters for models of supercooled water, which allows us to examine the possibility of two distinct metastable liquid phases [D. T. Limmer and D. Chandler, J. Chem. Phys.135, 134503 (2011) and preprint http://arxiv.org/abs/arXiv:1107.0337 (2011)]. Low-temperature reversible free energy surfaces of several different atomistic models are computed: mW water, TIP4P/2005 water, Stillinger-Weber silicon, and ST2 water, the last of these comparing three different treatments of long-ranged forces. In each case, we show that there is one stable or metastable liquid phase, and there is an ice-like crystal phase. The time scales for crystallization in these systems far exceed those of structural relaxation in the supercooled metastable liquid. We show how this wide separation in time scales produces an illusion of a low-temperature liquid-liquid transition. The phenomenon suggesting metastability of two distinct liquid phases is actually coarsening of the ordered ice-like phase, which we elucidate using both analytical theory and computer simulation. For the latter, we describe robust methods for computing reversible free energy surfaces, and we consider effects of electrostatic boundary conditions. We show that sensible alterations of models and boundary conditions produce no qualitative changes in low-temperature phase behaviors of these systems, only marginal changes in equations of state. On the other hand, we show that altering sampling time scales can produce large and qualitative non-equilibrium effects. Recent reports of evidence of a liquid-liquid critical point in computer simulations of supercooled water are considered in this light.

The putative liquid-liquid transition is a liquid-solid transition in atomistic models of water. II.

Science.gov (United States)

Limmer, David T; Chandler, David

2013-06-07

This paper extends our earlier studies of free energy functions of density and crystalline order parameters for models of supercooled water, which allows us to examine the possibility of two distinct metastable liquid phases [D. T. Limmer and D. Chandler, J. Chem. Phys. 135, 134503 (2011) and preprint arXiv:1107.0337 (2011)]. Low-temperature reversible free energy surfaces of several different atomistic models are computed: mW water, TIP4P/2005 water, Stillinger-Weber silicon, and ST2 water, the last of these comparing three different treatments of long-ranged forces. In each case, we show that there is one stable or metastable liquid phase, and there is an ice-like crystal phase. The time scales for crystallization in these systems far exceed those of structural relaxation in the supercooled metastable liquid. We show how this wide separation in time scales produces an illusion of a low-temperature liquid-liquid transition. The phenomenon suggesting metastability of two distinct liquid phases is actually coarsening of the ordered ice-like phase, which we elucidate using both analytical theory and computer simulation. For the latter, we describe robust methods for computing reversible free energy surfaces, and we consider effects of electrostatic boundary conditions. We show that sensible alterations of models and boundary conditions produce no qualitative changes in low-temperature phase behaviors of these systems, only marginal changes in equations of state. On the other hand, we show that altering sampling time scales can produce large and qualitative non-equilibrium effects. Recent reports of evidence of a liquid-liquid critical point in computer simulations of supercooled water are considered in this light.

Doping reversed-phase media for improved peptide purification.

Science.gov (United States)

Khalaf, Rushd; Forrer, Nicola; Buffolino, Gianluca; Gétaz, David; Bernardi, Susanna; Butté, Alessandro; Morbidelli, Massimo

2015-06-05

The purification of therapeutic peptides is most often performed using one or more reversed phase chromatography steps. This ensures high purities while keeping the costs of purification under control. In this paper, a doped reversed phase chromatographic material is tested and compared to traditional reversed phase materials. The doping consists of adding limited amounts of ion exchange ligands to the surface of the material to achieve orthogonal separation and increase the non-hydrophobic interactions with the surface. These ionic groups can either be attractive (opposite charge), or repulsive (same charge) to the peptide. The benefit of this new doped reversed phase material is shown through increases in selectivity in diluted conditions and yield and productivity in overloaded (i.e. industrial) conditions. It is the conjectured that all performance characteristics should increase using repulsive doping groups, whereas these characteristics should decrease when using attractive doping groups. This conjecture is shown to be true through several examples, including purifications of industrially relevant peptide crudes, in industrially relevant conditions. Moreover, the effect of ionic strength and organic modifier concentration was explored and shown to be in line with the expected behavior. Copyright © 2015 Elsevier B.V. All rights reserved.

Crystal-liquid-gas phase transitions and thermodynamic similarity

CERN Document Server

Skripov, Vladimir P; Schmelzer, Jurn W P

2006-01-01

Professor Skripov obtained worldwide recognition with his monograph ""Metastable liquids"", published in English by Wiley & Sons. Based upon this work and another monograph published only in Russia, this book investigates the behavior of melting line and the properties of the coexisting crystal and liquid phase of simple substances across a wide range of pressures, including metastable states of the coexisting phases. The authors derive new relations for the thermodynamic similarity for liquid-vapour phase transition, as well as describing solid-liquid, liquid-vapor and liquid-liquid phase tra

Analysis of electrophoretic soil humic acids fractions by reversed-phase high performance liquid chromatography with on-line absorbance and fluorescence detection.

Science.gov (United States)

Trubetskoj, Oleg A; Richard, Claire; Guyot, Ghislain; Voyard, Guillaume; Trubetskaya, Olga E

2012-06-22

A combination of reversed-phase high performance liquid chromatography (RP HPLC) with on-line absorbance and fluorescence detection was used for analysis of chernozem soil humic acids (HAs) and their fractions A, B and C+D with different electrophoretic mobility (EM) and molecular size (MS). Samples were injected onto the column at the identical volume and absorbance. All chromatograms exhibit the resolution of seven peaks. The estimation of relative recovery of HAs and fractions from the reverse-phase column has been done. High MS fraction A, which possesses the low EM, is essentially more hydrophobic (73% of the fraction amount remained adsorbed on the column) and aliphatic than medium MS and EM fraction B (33% of the fraction amount remained adsorbed on the column). The most hydrophilic and aromatic properties belong to low MS fraction C+D, which possess the highest EM and practically was not adsorbed on the column. The hydrophobicity of the bulk HAs lies within the range of fractions hydrophobicity. The absorption spectra of bulk HAs, electrophoretic fractions A, B, C+D and corresponding RP HPLC peaks were featureless but had differences in the values of absorbance ratio at 300 and 400 nm (A3/A4). For fractions A and B this ratio gradually decreased from peak 1 to 7 (from 3.05 to 2.80 and 3.00 to 2.40, respectively). This trend was less pronounced in HAs and practically absent in fraction C+D, where ratio A3/A4 varied within a small range. The strong relationship between fluorescence properties, EM, MS, polarity and aliphaticity/aromaticity of HAs fractions was found. Humic and protein-like fluorescence had different polarity nature. The protein-like fluorescence is located in humic material which irreversibly adsorbed on the reverse-phase column and not subjected to RP HPLC characterization. The humic-like fluorescence at Ex/Em 270/450 nm is mostly located in the hydrophilic peak of low MS fraction C+D. Taking into account that high MS fraction A consisted

Ultrasound extracted flavonoids from four varieties of Portuguese red grape skins determined by reverse-phase high-performance liquid chromatography with electrochemical detection.

Science.gov (United States)

Novak, Ivana; Janeiro, Patricia; Seruga, Marijan; Oliveira-Brett, Ana Maria

2008-12-23

Several flavonoids present in red grape skins from four varieties of Portuguese grapes were determined by reverse-phase high-performance liquid chromatography (RP-HPLC) with electrochemical detection (ECD). Extraction of flavonoids from red grape skins was performed by ultrasonication, and hydrochloric acid in methanol was used as extraction solvent. The developed RP-HPLC method used combined isocratic and gradient elution with amperometric detection with a glassy carbon-working electrode. Good peak resolution was obtained following direct injection of a sample of red grape extract in a pH 2.20 mobile phase. Eleven different flavonoids: cyanidin-3-O-glucoside (kuromanin), delphinidin-3-O-glucoside (myrtillin), petunidin-3-O-glucoside, peonidin-3-O-glucoside, malvidin-3-O-glucoside (oenin), (+)-catechin, rutin, fisetin, myricetin, morin and quercetin, can be separated in a single run by direct injection of sample solution. The limit of detection obtained for these compounds by ECD was 20-90 pg/L, 1000 times lower when compared with photodiode array (PDA) limit of detection of 12-55 ng/L. RP-HPLC-ECD was characterized by an excellent sensitivity and selectivity, and appropriate for the simultaneous determination of these electroactive phenolic compounds present in red grape skins.

Treatment of radioactive liquid waste by tubular type reverse osmosis module

International Nuclear Information System (INIS)

Nishimaki, Kenzo; Koyama, Akio; Tsutsui, Tenson; Mori, Koji.

1988-01-01

The applicability of reverse osmosis to radioactive liquid waste treatment was studied using a tubular type module. When four modules were used in a series, circulating volume of concentrate was much greater than permeate volume, therefore solute concentration and circulating rate of concentrate can be assumed uniform in the axial direction of the modules. DFs of stable elements contained in the tap water were 36-40 for Na, 50-55 for K, 170-250 for Mg and 90-160 for Ca. When Na concentration increased about ten times, DFs for all elements slightly decreased. For actual liquid waste tagged with radionuclides, DFs were in the range of 35-40 for 134 Cs, 150-200 for 85 Sr, and 180-280 for 58 Co. These DF values indicate the possibility of the treatment of low radioactive liquid waste by reverse osmosis. (author)

Systematic evaluation of matrix effects in hydrophilic interaction chromatography versus reversed phase liquid chromatography coupled to mass spectrometry.

Science.gov (United States)

Periat, Aurélie; Kohler, Isabelle; Thomas, Aurélien; Nicoli, Raul; Boccard, Julien; Veuthey, Jean-Luc; Schappler, Julie; Guillarme, Davy

2016-03-25

Reversed phase liquid chromatography (RPLC) coupled to mass spectrometry (MS) is the gold standard technique in bioanalysis. However, hydrophilic interaction chromatography (HILIC) could represent a viable alternative to RPLC for the analysis of polar and/or ionizable compounds, as it often provides higher MS sensitivity and alternative selectivity. Nevertheless, this technique can be also prone to matrix effects (ME). ME are one of the major issues in quantitative LC-MS bioanalysis. To ensure acceptable method performance (i.e., trueness and precision), a careful evaluation and minimization of ME is required. In the present study, the incidence of ME in HILIC-MS/MS and RPLC-MS/MS was compared for plasma and urine samples using two representative sets of 38 pharmaceutical compounds and 40 doping agents, respectively. The optimal generic chromatographic conditions in terms of selectivity with respect to interfering compounds were established in both chromatographic modes by testing three different stationary phases in each mode with different mobile phase pH. A second step involved the assessment of ME in RPLC and HILIC under the best generic conditions, using the post-extraction addition method. Biological samples were prepared using two different sample pre-treatments, i.e., a non-selective sample clean-up procedure (protein precipitation and simple dilution for plasma and urine samples, respectively) and a selective sample preparation, i.e., solid phase extraction for both matrices. The non-selective pretreatments led to significantly less ME in RPLC vs. HILIC conditions regardless of the matrix. On the contrary, HILIC appeared as a valuable alternative to RPLC for plasma and urine samples treated by a selective sample preparation. Indeed, in the case of selective sample preparation, the compounds influenced by ME were different in HILIC and RPLC, and lower and similar ME occurrence was generally observed in RPLC vs. HILIC for urine and plasma samples

Quantitative structure-retention relationships of pesticides in reversed-phase high-performance liquid chromatography based on WHIM and GETAWAY molecular descriptors

Energy Technology Data Exchange (ETDEWEB)

D' Archivio, Angelo Antonio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)], E-mail: darchivi@univaq.it; Maggi, Maria Anna; Mazzeo, Pietro; Ruggieri, Fabrizio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)

2008-11-03

The ability of the Weighted Holistic Invariant Molecular (WHIM) and GEometry, Topology, and Atom-Weights AssemblY (GETAWAY) descriptors to represent the effect of molecular structure on the retention of pesticides in reversed-phase high-performance liquid chromatography (RP-HPLC) is investigated. To this end, two retention data sets previously collected in water-acetonitrile mobile phase are re-examined. The first data set (data-set-1) consists of retention data of 26 neutral compounds belonging to widely used pesticide classes, collected within the mobile phase composition range 40-65% (v/v) acetonitrile. The second data set (data-set-2) describes retention of phenoxy acid herbicides and structurally related compounds (benzoic acid and phenylacetic acid derivatives), as a whole covering the pK{sub a} range 2.3-4.3, as a function of mobile phase composition, ranging between 30 and 70% (v/v) acetonitrile, and pH, ranging between 2 and 5. For each data set, the mobile phase attributes are combined with WHIM or GETAWAY descriptors into 'mixed' predictive models in order to attempt retention modelling within the whole mobile phase composition range of analytical interest. Six- or seven-dimensional multilinear models, preliminarily selected using a genetic algorithm, were improved using a multi-layer artificial neural network (ANN) learned by back propagation. ANN performance was tested on three molecules not used in the learning stage and by leave-more-out cross validation. The results reveal that while WHIM descriptors seem not adequate to model retention of solutes of data-set-1, GETAWAY descriptors provide a satisfactory retention model. On the other hand WHIM and GETAWAY descriptors applied to data-set-2 provide a similar performance, even if slightly worse as compared with the above case. Accuracy of retention modelling in these cases is comparable or slightly poorer as compared with the results previously obtained by combining quantum chemical

Quantitative structure-retention relationships of pesticides in reversed-phase high-performance liquid chromatography based on WHIM and GETAWAY molecular descriptors

International Nuclear Information System (INIS)

D'Archivio, Angelo Antonio; Maggi, Maria Anna; Mazzeo, Pietro; Ruggieri, Fabrizio

2008-01-01

The ability of the Weighted Holistic Invariant Molecular (WHIM) and GEometry, Topology, and Atom-Weights AssemblY (GETAWAY) descriptors to represent the effect of molecular structure on the retention of pesticides in reversed-phase high-performance liquid chromatography (RP-HPLC) is investigated. To this end, two retention data sets previously collected in water-acetonitrile mobile phase are re-examined. The first data set (data-set-1) consists of retention data of 26 neutral compounds belonging to widely used pesticide classes, collected within the mobile phase composition range 40-65% (v/v) acetonitrile. The second data set (data-set-2) describes retention of phenoxy acid herbicides and structurally related compounds (benzoic acid and phenylacetic acid derivatives), as a whole covering the pK a range 2.3-4.3, as a function of mobile phase composition, ranging between 30 and 70% (v/v) acetonitrile, and pH, ranging between 2 and 5. For each data set, the mobile phase attributes are combined with WHIM or GETAWAY descriptors into 'mixed' predictive models in order to attempt retention modelling within the whole mobile phase composition range of analytical interest. Six- or seven-dimensional multilinear models, preliminarily selected using a genetic algorithm, were improved using a multi-layer artificial neural network (ANN) learned by back propagation. ANN performance was tested on three molecules not used in the learning stage and by leave-more-out cross validation. The results reveal that while WHIM descriptors seem not adequate to model retention of solutes of data-set-1, GETAWAY descriptors provide a satisfactory retention model. On the other hand WHIM and GETAWAY descriptors applied to data-set-2 provide a similar performance, even if slightly worse as compared with the above case. Accuracy of retention modelling in these cases is comparable or slightly poorer as compared with the results previously obtained by combining quantum chemical descriptors or usual

A rapid monitoring method for inorganic arsenic in rice flour using reversed phase-high performance liquid chromatography-inductively coupled plasma mass spectrometry.

Science.gov (United States)

Narukawa, Tomohiro; Chiba, Koichi; Sinaviwat, Savarin; Feldmann, Jörg

2017-01-06

A new rapid monitoring method by means of high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) following the heat-assisted extraction was developed for measurement of total inorganic arsenic species in rice flour. As(III) and As(V) eluted at the same retention time and completely separated from organoarsenic species by an isocratic elution program on a reversed phase column. Therefore, neither ambiguous oxidation of arsenite to arsenate nor the integration of two peaks were necessary to determine directly the target analyte inorganic arsenic. Rapid injection allowed measuring 3 replicates within 6min and this combined with a quantitative extraction of all arsenic species from rice flour by a 15min HNO 3 -H 2 O 2 extraction makes this the fastest laboratory based method for inorganic arsenic in rice flour. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of large volume injection of aliphatic alcohols as sample diluents on the retention of low hydrophobic solutes in reversed-phase liquid chromatography.

Science.gov (United States)

David, Victor; Galaon, Toma; Aboul-Enein, Hassan Y

2014-01-03

Recent studies showed that injection of large volume of hydrophobic solvents used as sample diluents could be applied in reversed-phase liquid chromatography (RP-LC). This study reports a systematic research focused on the influence of a series of aliphatic alcohols (from methanol to 1-octanol) on the retention process in RP-LC, when large volumes of sample are injected on the column. Several model analytes with low hydrophobic character were studied by RP-LC process, for mobile phases containing methanol or acetonitrile as organic modifiers in different proportions with aqueous component. It was found that starting with 1-butanol, the aliphatic alcohols can be used as sample solvents and they can be injected in high volumes, but they may influence the retention factor and peak shape of the dissolved solutes. The dependence of the retention factor of the studied analytes on the injection volume of these alcohols is linear, with a decrease of its value as the sample volume is increased. The retention process in case of injecting up to 200μL of upper alcohols is dependent also on the content of the organic modifier (methanol or acetonitrile) in mobile phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Role of Reversible Phase Transformation for Strong Piezoelectric Performance at the Morphotropic Phase Boundary

Science.gov (United States)

Liu, Hui; Chen, Jun; Huang, Houbing; Fan, Longlong; Ren, Yang; Pan, Zhao; Deng, Jinxia; Chen, Long-Qing; Xing, Xianran

2018-01-01

A functional material with coexisting energetically equivalent phases often exhibits extraordinary properties such as piezoelectricity, ferromagnetism, and ferroelasticity, which is simultaneously accompanied by field-driven reversible phase transformation. The study on the interplay between such phase transformation and the performance is of great importance. Here, we have experimentally revealed the important role of field-driven reversible phase transformation in achieving enhanced electromechanical properties using in situ high-energy synchrotron x-ray diffraction combined with 2D geometry scattering technology, which can establish a comprehensive picture of piezoelectric-related microstructural evolution. High-throughput experiments on various Pb /Bi -based perovskite piezoelectric systems suggest that reversible phase transformation can be triggered by an electric field at the morphotropic phase boundary and the piezoelectric performance is highly related to the tendency of electric-field-driven phase transformation. A strong tendency of phase transformation driven by an electric field generates peak piezoelectric response. Further, phase-field modeling reveals that the polarization alignment and the piezoelectric response can be much enhanced by the electric-field-driven phase transformation. The proposed mechanism will be helpful to design and optimize the new piezoelectrics, ferromagnetics, or other related functional materials.

Analysis of metallic nanoparticles and their ionic counterparts in complex matrix by reversed-phase liquid chromatography coupled to ICP-MS.

Science.gov (United States)

Yang, Yuan; Luo, Li; Li, Hai-Pu; Wang, Qiang; Yang, Zhao-Guang; Qu, Zhi-Peng; Ding, Ru

2018-05-15

Developing quantification and characterization methodology for metallic nanoparticles (MNPs) and their ionic component in complex matrix are crucial for the evaluation of their environmental behavior and health risks to humans. In this study, reversed phase high performance liquid chromatography combined ICP-MS was established for the characterization of MNPs in complex matrix. The ionic component could be separated from NPs with the optimized parameters of aqueous mobile phase. Good linear relationship between average diameter and retention time of NPs was obtained using HPLC-ICP-MS and the size smaller than 40 nm could be determined with this method, the detected results were in accordance with TEM results. The low detection limit of AuNPs and Au(Ⅲ) (both in sub-μg/L level) showed that this method was promising for the characterization of AuNPs and Au(Ⅲ) in environmental water. The mass concentration of ionic Au(Ⅲ) in environmental water could be detected using the proposed HPLC-ICP-MS and the concentration of AuNPs was obtained by subtracting the Au(Ⅲ) concentration from the total Au (The concentration of total Au was detected by ICP-MS after microwave digestion). Furthermore this proposed HPLC-ICP-MS method and single particle-ICPMS (SP-ICP-MS) was used for the analysis of the Ag speciation in commercial antibacterial products. Copyright © 2018 Elsevier B.V. All rights reserved.

Study of pH dependence using molecular modeling in reversed-phase liquid chromatography of 1-phenyl-3-methyl-5-pyrazolone derivatives of aldose

International Nuclear Information System (INIS)

Yamamoto, Fumiko M.; Rokushika, Souji

2004-01-01

A series of 1-phenyl-3-methyl-5-pyrazolone (PMP) aldose was eluted on a C 18 column with an acetonitrile-phosphate buffer over the range of pH 2-10 in reversed phase liquid chromatography. The relationship between the retention factor, k, and the eluent pH was expressed by an equilibrium scheme representing the probable retention process. The experimental data were fitted to the correlation curve drawn according to the equation containing the formation of the hydrogen bond with a hydroxonium ion in the eluent and the ionization of the oxygen atoms in the pyrazolone rings of the solute. The conformational changes of PMP-aldose according with the eluent pH were corroborated by computer-aided molecular modeling using quantum chemical calculations. The retention behavior was elucidated as a function of the geometrical feature of the PMP-aldose

Determination of reversed-phase high performance liquid chromatography based octanol-water partition coefficients for neutral and ionizable compounds: Methodology evaluation.

Science.gov (United States)

Liang, Chao; Qiao, Jun-Qin; Lian, Hong-Zhen

2017-12-15

Reversed-phase liquid chromatography (RPLC) based octanol-water partition coefficient (logP) or distribution coefficient (logD) determination methods were revisited and assessed comprehensively. Classic isocratic and some gradient RPLC methods were conducted and evaluated for neutral, weak acid and basic compounds. Different lipophilicity indexes in logP or logD determination were discussed in detail, including the retention factor logk w corresponding to neat water as mobile phase extrapolated via linear solvent strength (LSS) model from isocratic runs and calculated with software from gradient runs, the chromatographic hydrophobicity index (CHI), apparent gradient capacity factor (k g ') and gradient retention time (t g ). Among the lipophilicity indexes discussed, logk w from whether isocratic or gradient elution methods best correlated with logP or logD. Therefore logk w is recommended as the preferred lipophilicity index for logP or logD determination. logk w easily calculated from methanol gradient runs might be the main candidate to replace logk w calculated from classic isocratic run as the ideal lipophilicity index. These revisited RPLC methods were not applicable for strongly ionized compounds that are hardly ion-suppressed. A previously reported imperfect ion-pair RPLC method was attempted and further explored for studying distribution coefficients (logD) of sulfonic acids that totally ionized in the mobile phase. Notably, experimental logD values of sulfonic acids were given for the first time. The IP-RPLC method provided a distinct way to explore logD values of ionized compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Prediction of the retention of s-triazines in reversed-phase high-performance liquid chromatography under linear gradient-elution conditions.

Science.gov (United States)

D'Archivio, Angelo Antonio; Maggi, Maria Anna; Ruggieri, Fabrizio

2014-08-01

In this paper, a multilayer artificial neural network is used to model simultaneously the effect of solute structure and eluent concentration profile on the retention of s-triazines in reversed-phase high-performance liquid chromatography under linear gradient elution. The retention data of 24 triazines, including common herbicides and their metabolites, are collected under 13 different elution modes, covering the following experimental domain: starting acetonitrile volume fraction ranging between 40 and 60% and gradient slope ranging between 0 and 1% acetonitrile/min. The gradient parameters together with five selected molecular descriptors, identified by quantitative structure-retention relationship modelling applied to individual separation conditions, are the network inputs. Predictive performance of this model is evaluated on six external triazines and four unseen separation conditions. For comparison, retention of triazines is modelled by both quantitative structure-retention relationships and response surface methodology, which describe separately the effect of molecular structure and gradient parameters on the retention. Although applied to a wider variable domain, the network provides a performance comparable to that of the above "local" models and retention times of triazines are modelled with accuracy generally better than 7%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mixed reverse micelles facilitated downstream processing of lipase involving water-oil-water liquid emulsion membrane.

Science.gov (United States)

Bhowal, Saibal; Priyanka, B S; Rastogi, Navin K

2014-01-01

Our earlier work for the first time demonstrated that liquid emulsion membrane (LEM) containing reverse micelles could be successfully used for the downstream processing of lipase from Aspergillus niger. In the present work, we have attempted to increase the extraction and purification fold of lipase by using mixed reverse micelles (MRM) consisting of cationic and nonionic surfactants in LEM. It was basically prepared by addition of the internal aqueous phase solution to the organic phase followed by the redispersion of the emulsion in the feed phase containing enzyme, which resulted in globules of water-oil-water (WOW) emulsion for the extraction of lipase. The optimum conditions for maximum lipase recovery (100%) and purification fold (17.0-fold) were CTAB concentration 0.075 M, Tween 80 concentration 0.012 M, at stirring speed of 500 rpm, contact time 15 min, internal aqueous phase pH 7, feed pH 9, KCl concentration 1 M, NaCl concentration 0.1 M, and ratio of membrane emulsion to feed volume 1:1. Incorporation of the nonionic surfactant (e.g., Tween 80) resulted in remarkable improvement in the purification fold (3.1-17.0) of the lipase. LEM containing a mixture of nonionic and cationic surfactants can be successfully used for the enhancement in the activity recovery and purification fold during downstream processing of enzymes/proteins. © 2014 American Institute of Chemical Engineers.

Simultaneous determination of secondary metabolites from Vinca rosea plant extractives by reverse phase high performance liquid chromatography

Science.gov (United States)

Siddiqui, Mohammad Jamshed Ahmad; Ismail, Zhari; Saidan, Noor Hafizoh

2011-01-01

Background: Vinca rosea (Apocynaceae) is one of the most important and high value medicinal plants known for its anticancer alkaloids. It is the iota of the isolated secondary metabolites used in chemotherapy to treat diverse cancers. Several high performance liquid chromatography (HPLC) methods have been developed to quantify the active alkaloids in the plant. However, this method may serve the purpose in quantification of V. rosea plant extracts in totality. Objective: To develop and validate the reverse phase (RP)-HPLC method for simultaneous determination of secondary metabolites, namely alkaloids from V. rosea plant extracts. Materials and Methods: The quantitative determination was conducted by RP-HPLC equipped with ultraviolet detector. Optimal separation was achieved by isocratic elution with mobile phase consisting of methanol:acetonitrile:ammonium acetate buffer (25 mM) with 0.1% triethylamine (15:45:40 v/v) on a column (Zorbax Eclipse plus C18, 250 mm % 4.6 mm; 5 μm). The standard markers (vindoline, vincristine, catharanthine, and vinblastine) were identified by retention time and co-injected with reference standard and quantified by external standard method at 297 nm. Results: The precision of the method was confirmed by the relative standard deviation (R.S.D.), which was lower than 2.68%. The recoveries were in the range of 98.09%-108%. The limits of detection (LOD) for each marker alkaloids were lower than 0.20 μg. Different parts of the V. rosea extracts shows different concentrations of markers, flower samples were high in vinblastine content, while methanol extract from the leaves contains all the four alkaloids in good yield, and there is no significant presence of markers in water extracts. Conclusion: HPLC method established is appropriate for the standardization and quality assurance of V. rosea plant extracts. PMID:21716929

Reversible, on-demand generation of aqueous two-phase microdroplets

Science.gov (United States)

Collier, Charles Patrick; Retterer, Scott Thomas; Boreyko, Jonathan Barton; Mruetusatorn, Prachya

2017-08-15

The present invention provides methods of on-demand, reversible generation of aqueous two-phase microdroplets core-shell microbeads, microparticle preparations comprising the core-shell microbeads, and drug delivery formulation comprising the microparticle preparations. Because these aqueous microdroplets have volumes comparable to those of cells, they provide an approach to mimicking the dynamic microcompartmentation of biomaterial that naturally occurs within the cytoplasm of cells. Hence, the present methods generate femtoliter aqueous two-phase droplets within a microfluidic oil channel using gated pressure pulses to generate individual, stationary two-phase microdroplets with a well-defined time zero for carrying out controlled and sequential phase transformations over time. Reversible phase transitions between single-phase, two-phase, and core-shell microbead states are obtained via evaporation-induced dehydration and water rehydration.

Supported ionic liquid-phase (SILP) catalysis

DEFF Research Database (Denmark)

Riisager, Anders; Fehrmann, Rasmus; Wasserscheid, P.

2005-01-01

The concept of supported ionic liquid-phase (SILP) catalysis has been demonstrated for gas- and liquid-phase continuous fixed-bed reactions using rhodium phosphine catalyzed hydroformylation of propene and 1-octene as examples. The nature of the support had important influence on both the catalytic...

A Simple and Validated Reverse Phase HPLC Methodfor the Determination of Rabeprazole inPharmaceutical Dosage Forms

Directory of Open Access Journals (Sweden)

Uma Mahesh Karra

2010-01-01

Full Text Available A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC method was developed and validated for quantitative determination of rabeprazole in bulk drug samples and formulations. Rabeprazole was analyzed by using reverse phase LC-GC column (Inertsil ODS, 4.6 mm x 25 cm, 5 microns, with mobile phase consisting of methanol: water (78:22 v/v. The flow rate was set 1.0 mL/min and analysis was performed at wavelength 288 nm using Photo Diode Array (PDA detector at ambient temperature. The method was validated and stability studies were conducted under different conditions. The retention time for rabeprazole was around 4.12 minutes. The calibration curves were linear (r≥0.9998 over a concentration range from 20.0 to 80.0 μg/mL. Limit of detection (LOD and Limit of quantitation (LOQ were 8 ng/mL and 24 ng/mL respectively. The developed method was successfully applied to estimate the amount of rabeprazole in tablet formulations.

Kinetics and reversibility of radiocaesium solid/liquid partitioning in sediments

International Nuclear Information System (INIS)

Comans, R.N.J.

1998-01-01

The kinetics and reversibility of radiocaesium solid/liquid partitioning in sediments have been reviewed and interpreted in terms of a mechanistic framework. This framework is based on the premise that radiocaesium is almost exclusively and highly-selectively bound to the frayed particle edges of illitic clay minerals in the sediments. Several processes with distinctly different rates can be distinguished in radiocaesium sorption to sediments. 2- and 3-box kinetic models can describe both the overall solid/liquid partitioning in sediments and the reversible (exchangeable) and irreversible (nonexchangeable or 'fixed') fractions of radiocaesium in sediments over time scales relevant for natural aquatic systems. The obtained rate parameters indicate that reversible partitioning of radiocaesium dominates over the first few days following a contamination event, whereas irreversible kinetics becomes important over time scales of weeks to months. The slow process, which reduces the exchangeability of sediment-bound radiocaesium over time, is believed to result from a migration of radiocaesium from exchangeable sites on the frayed edges of illite towards less-exchangeable interlayer sites. Long-term extraction of radiocaesium from historically contaminated sediments has given evidence for a reverse (remobilization) process with a half-life of the order of tens of years. These findings suggest that the long-term exchangeability of radiocaesium in sediments may be higher than the few % which is generally assumed. (orig.)

Determination of the n-octanol/water partition coefficients of weakly ionizable basic compounds by reversed-phase high-performance liquid chromatography with neutral model compounds.

Science.gov (United States)

Liang, Chao; Han, Shu-ying; Qiao, Jun-qin; Lian, Hong-zhen; Ge, Xin

2014-11-01

A strategy to utilize neutral model compounds for lipophilicity measurement of ionizable basic compounds by reversed-phase high-performance liquid chromatography is proposed in this paper. The applicability of the novel protocol was justified by theoretical derivation. Meanwhile, the linear relationships between logarithm of apparent n-octanol/water partition coefficients (logKow '') and logarithm of retention factors corresponding to the 100% aqueous fraction of mobile phase (logkw ) were established for a basic training set, a neutral training set and a mixed training set of these two. As proved in theory, the good linearity and external validation results indicated that the logKow ''-logkw relationships obtained from a neutral model training set were always reliable regardless of mobile phase pH. Afterwards, the above relationships were adopted to determine the logKow of harmaline, a weakly dissociable alkaloid. As far as we know, this is the first report on experimental logKow data for harmaline (logKow = 2.28 ± 0.08). Introducing neutral compounds into a basic model training set or using neutral model compounds alone is recommended to measure the lipophilicity of weakly ionizable basic compounds especially those with high hydrophobicity for the advantages of more suitable model compound choices and convenient mobile phase pH control. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystalline liquids: the blue phases

Science.gov (United States)

Wright, David C.; Mermin, N. David

1989-04-01

The blue phases of cholesteric liquid crystals are liquids that exhibit orientational order characterized by crystallographic space-group symmetries. We present here a pedagogical introduction to the current understanding of the equilibrium structure of these phases accompanied by a general overview of major experimental results. Using the Ginzburg-Landau free energy appropriate to the system, we first discuss in detail the character and stability of the usual helical phase of cholesterics, showing that for certain parameter ranges the helical phase is unstable to the appearance of one or more blue phases. The two principal models for the blue phases are two limiting cases of the Ginzburg-Landau theory. We explore each limit and conclude with some general considerations of defects in both models and an exact minimization of the free energy in a curved three-dimensional space.

An analysis of dissolved organic matter from freshwater Karelian Lakes using reversed-phase high-performance liquid chromatography with online absorbance and fluorescence analysis

Science.gov (United States)

Khundzhua, D. A.; Patsaeva, S. V.; Trubetskoj, O. A.; Trubetskaya, O. E.

2017-01-01

The spectral and optical properties of the fractionated components of dissolved organic matter (DOM) of three freshwater lakes in Karelia were studied using reversed-phase high-performance liquid chromatography (RP-HPLC) with online detection of fluorescence and absorption spectra. It is shown that the DOM fractions are qualitatively similar, but differ quantitatively in the ratio of components and consist of at least three types of fluorophores: (1) hydrophilic "humic-like" fluorophore(s) with the emission maximum in the region of 420 nm and an absorption band at 260-270 nm; (2) hydrophobic "humic-like" fluorophore(s) with the emission maximum at approximately 450 nm that has no characteristic absorption maxima in the region from 220 to 400 nm; and (3) a "protein-like" fluorophore with the emission maximum in the region of 340-350 nm, which is typical of proteins and peptides containing tryptophan.

Determination of phenolic derivatives of antipyrine in plasma with solid-phase extraction and high-performance liquid chromatography-atmospheric-pressure chemical ionization mass spectrometry

NARCIS (Netherlands)

Coolen, S.A.J.; Ligor, T.; Lieshout, van H.P.M.; Huf, F.A.

1999-01-01

This manuscript describes a method to determine antipyrine and its phenolic derivatives in plasma by reversed-phase high-performance liquid chromatography–mass spectrometry (RP-HPLC–MS). The sample pretreatment consisted of a C18 solid-phase extraction (SPE), to remove the salts and proteins. The

Determination of acetone in saliva by reversed-phase liquid chromatography with fluorescence detection and the monitoring of diabetes mellitus patients with ketoacidosis.

Science.gov (United States)

Fujii, Shinya; Maeda, Toshio; Noge, Ichiro; Kitagawa, Yutaka; Todoroki, Kenichiro; Inoue, Koichi; Min, Jun Zhe; Toyo'oka, Toshimasa

2014-03-20

In diabetes mellitus (DM) patients with ketoacidosis, ketone bodies, i.e., acetone, acetoacetic acid (AA) and β-hydroxybutyric acid (HA), are increased in the blood and urine. Acetone is also excreted by breathing due to the spontaneous decomposition of AA. Thus, the increase in acetone has been considered as one of the biomarkers for the diagnosis of DM. However, the determination of acetone in one's breath is not recommended because of the sample handling difficulty. We measured acetone in saliva by reversed-phase liquid chromatography (LC) with fluorescence (FL) detection. The proposed method was applied to the determination of acetone in the saliva of healthy volunteers and DM patients with and without ketoacidosis. 3-Pentanone (I.S.) and DBD-H in acetonitrile were added to freshly collected saliva and reacted at room temperature for 20 min in the presence of trifluoroacetic acid. After the reaction, the solution was centrifuged at 10,000 × g and 4 °C for 5 min. The supernatant was separated by reversed-phase LC and the FL detected at 550 nm (excitation at 460 nm). The concentrations of acetone in the DM patients with ketoacidosis were significantly higher than those of the normal subjects and DM patients without ketoacidosis. Furthermore, the total contents of the ketone bodies in the blood correlated with acetone in the saliva of the DM patients. The concentrations of acetone in the saliva of an emergency patient also correlated with the ketone bodies in the blood at each sampling time. The proposed method using LC-FL seems to be useful for the determination of acetone in the saliva of DM patients with ketoacidosis. The method offers a new option for the diagnosis and monitoring of DM patients with ketoacidosis. Copyright © 2014 Elsevier B.V. All rights reserved.

Develop and validation of an analytic method for the histamine determination in fish, using chromatography liquidates of high efficiency in reverse phase with ultraviolet detection

International Nuclear Information System (INIS)

Valverde Chavarria, J. C.

1997-01-01

There were determined and optimized the reaction and conditions analysis, for the derivation of the histamine with the reagent of or-ftalaldehido (OPA), it was proven that it is possible to quantify the one derived formed at 333nm. The good conditions crhomatografics settled down for the determination of the histamine in fish by means of the analytic technique of chromatography it liquidates of high efficiency (HPLC) in reverse phase, using the derivatizacion in precolumn of the histamine with the reagent of OPA, with ultraviolet detection at 333nm. The conditions of the proposed methodology were optimized and the variables of analytic acting were validated, for the analytic quantification of the histamine in the mg g-1 environment. The applicability of the methodology was demonstrated in the histamine determination in samples of fresh fish [es

A reversed-phase high performance liquid chromatography coupled with resonance Rayleigh scattering detection for the determination of four tetracycline antibiotics

International Nuclear Information System (INIS)

Wang Lifeng; Peng Jingdong; Liu Limin

2008-01-01

A new reversed-phase high performance liquid chromatography with resonance Rayleigh scattering detection (HPLC-RRS) was developed for simultaneous separation and determination of four tetracycline antibiotics (TCs). A good chromatographic separation among the compounds was achieved using a Synergi Fusion-RP column (150 mm x 4.6 mm; 4 μm) and a mobile phase consisting of methanol-acetonitrile-oxalic acid (5 mM) at the flow rate of 0.8 mL min -1 . Column temperature was 30 deg. C. The RRS signal was detected at λ ex = λ em = 370 nm. The recoveries of sample added standard ranged from 95.3% to 103.5%, and the relative standard deviation was below 2.79%. A detection limit of 2.12-5.12 μg mL -1 was reached and a linear range was found between peak height and concentration in the range of 10.36-518.0 μg mL -1 for oxytetracycline (OTC), 12.11-605.5 μg mL -1 for tetracycline (TC), 11.79-589.5 μg mL -1 for chlortetracycline (CTC) and 10.32-516.0 μg mL -1 for doxycycline (DC). The linear regression coefficients were all above 0.999. The method has been applied successfully to the determination of OTC, TC, CTC, DC in pharmaceutical formulations and in honey. The method was simple, rapid and showed a better linear relation and high repeatability

A reversed-phase high performance liquid chromatography coupled with resonance Rayleigh scattering detection for the determination of four tetracycline antibiotics

Energy Technology Data Exchange (ETDEWEB)

Lifeng, Wang [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Peng Jingdong [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)], E-mail: hxpengjd@swu.edu.cn; Limin, Liu [School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China)

2008-12-07

A new reversed-phase high performance liquid chromatography with resonance Rayleigh scattering detection (HPLC-RRS) was developed for simultaneous separation and determination of four tetracycline antibiotics (TCs). A good chromatographic separation among the compounds was achieved using a Synergi Fusion-RP column (150 mm x 4.6 mm; 4 {mu}m) and a mobile phase consisting of methanol-acetonitrile-oxalic acid (5 mM) at the flow rate of 0.8 mL min{sup -1}. Column temperature was 30 deg. C. The RRS signal was detected at {lambda}{sub ex} = {lambda}{sub em} = 370 nm. The recoveries of sample added standard ranged from 95.3% to 103.5%, and the relative standard deviation was below 2.79%. A detection limit of 2.12-5.12 {mu}g mL{sup -1} was reached and a linear range was found between peak height and concentration in the range of 10.36-518.0 {mu}g mL{sup -1} for oxytetracycline (OTC), 12.11-605.5 {mu}g mL{sup -1} for tetracycline (TC), 11.79-589.5 {mu}g mL{sup -1} for chlortetracycline (CTC) and 10.32-516.0 {mu}g mL{sup -1} for doxycycline (DC). The linear regression coefficients were all above 0.999. The method has been applied successfully to the determination of OTC, TC, CTC, DC in pharmaceutical formulations and in honey. The method was simple, rapid and showed a better linear relation and high repeatability.

A simple, sensitive and rapid isocratic reversed-phase high-performance liquid chromatography method for determination and stability study of curcumin in pharmaceutical samples

Science.gov (United States)

Amanolahi, Farjad; Mohammadi, Ali; Kazemi Oskuee, Reza; Nassirli, Hooriyeh; Malaekeh-Nikouei, Bizhan

2017-01-01

Objective: This study was designed to develop and validate a new reversed-phase high-performance liquid chromatography (RP-HPLC) method based on Q2 (R1) International Conference on Harmonization (ICH) guideline for determination of curcumin in pharmaceutical samples. Materials and Methods: The HPLC instrument method was optimized with isocratic elution with acetonitrile: ammonium acetate (45:55, v/v, pH 3.5), C18 column (150 mm×4.6 mm×5 µm particle size) and a flow rate of 1 ml/min in ambient condition and total retention time of 17 min. The volume of injection was set at 20 µl and detection was recorded at 425 nm. The robustness of the method was examined by changing the mobile phase composition, mobile phase pH, and flow rate. Results: The method was validated with respect to precision, accuracy and linearity in a concentration range of 2-100 µg/ml. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 and 0.5 µg/ml, respectively. The percentage of recovery was 98.9 to 100.5 with relative standard deviation (RSD) < 0.638%. Conclusion: The method was found to be simple, sensitive and rapid for determination of curcumin in pharmaceutical samples and had enough sensitivity to detect degradation product of curcumin produced under photolysis and hydrolysis stress condition. PMID:29062806

SOLVENT EFFECTS IN THE LIQUID-PHASE HYDRATION OF CYCLOHEXENE CATALYZED BY A MACROPOROUS STRONG ACID ION-EXCHANGE RESIN

NARCIS (Netherlands)

PANNEMAN, HJ; BEENACKERS, AACM

1992-01-01

The liquid-phase hydration of cyclohexene, a pseudo first order reversible reaction catalyzed by a strong acid ion exchange resin, macroporous Amberlite XE 307, was investigated in solvent mixtures of water and sulfolane. A decrease by a factor of 3 and 6 is observed in the experimentally measured

Phase transitions in liquids with directed intermolecular bonding

OpenAIRE

Son, L.; Ryltcev, R.

2005-01-01

Liquids with quasi - chemical bonding between molecules are described in terms of vertex model. It is shown that this bonding results in liquid - liquid phase transition, which occurs between phases with different mean density of intermolecular bonds. The transition may be suggested to be a universal phenomena for those liquids.

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

Directory of Open Access Journals (Sweden)

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.

Phase stability analysis of liquid-liquid equilibrium with stochastic methods

Directory of Open Access Journals (Sweden)

G. Nagatani

2008-09-01

Full Text Available Minimization of Gibbs free energy using activity coefficient models and nonlinear equation solution techniques is commonly applied to phase stability problems. However, when conventional techniques, such as the Newton-Raphson method, are employed, serious convergence problems may arise. Due to the existence of multiple solutions, several problems can be found in modeling liquid-liquid equilibrium of multicomponent systems, which are highly dependent on the initial guess. In this work phase stability analysis of liquid-liquid equilibrium is investigated using the NRTL model. For this purpose, two distinct stochastic numerical algorithms are employed to minimize the tangent plane distance of Gibbs free energy: a subdivision algorithm that can find all roots of nonlinear equations for liquid-liquid stability analysis and the Simulated Annealing method. Results obtained in this work for the two stochastic algorithms are compared with those of the Interval Newton method from the literature. Several different binary and multicomponent systems from the literature were successfully investigated.

Liquid-liquid phase transition and glass transition in a monoatomic model system.

Science.gov (United States)

Xu, Limei; Buldyrev, Sergey V; Giovambattista, Nicolas; Stanley, H Eugene

2010-01-01

We review our recent study on the polyamorphism of the liquid and glass states in a monatomic system, a two-scale spherical-symmetric Jagla model with both attractive and repulsive interactions. This potential with a parametrization for which crystallization can be avoided and both the glass transition and the liquid-liquid phase transition are clearly separated, displays water-like anomalies as well as polyamorphism in both liquid and glassy states, providing a unique opportunity to study the interplay between the liquid-liquid phase transition and the glass transition. Our study on a simple model may be useful in understanding recent studies of polyamorphism in metallic glasses.

Liquid-Liquid Phase Transition and Glass Transition in a Monoatomic Model System

Directory of Open Access Journals (Sweden)

Nicolas Giovambattista

2010-12-01

Full Text Available We review our recent study on the polyamorphism of the liquid and glass states in a monatomic system, a two-scale spherical-symmetric Jagla model with both attractive and repulsive interactions. This potential with a parametrization for which crystallization can be avoided and both the glass transition and the liquid-liquid phase transition are clearly separated, displays water-like anomalies as well as polyamorphism in both liquid and glassy states, providing a unique opportunity to study the interplay between the liquid-liquid phase transition and the glass transition. Our study on a simple model may be useful in understanding recent studies of polyamorphism in metallic glasses.

Lyotropic liquid crystalline phase behaviour in amphiphile-protic ionic liquid systems.

Science.gov (United States)

Chen, Zhengfei; Greaves, Tamar L; Fong, Celesta; Caruso, Rachel A; Drummond, Calum J

2012-03-21

Approximate partial phase diagrams for nine amphiphile-protic ionic liquid (PIL) systems have been determined by synchrotron source small angle X-ray scattering, differential scanning calorimetry and cross polarised optical microscopy. The binary phase diagrams of some common cationic (hexadecyltrimethyl ammonium chloride, CTAC, and hexadecylpyridinium bromide, HDPB) and nonionic (polyoxyethylene (10) oleyl ether, Brij 97, and Pluronic block copolymer, P123) amphiphiles with the PILs, ethylammonium nitrate (EAN), ethanolammonium nitrate (EOAN) and diethanolammonium formate (DEOAF), have been studied. The phase diagrams were constructed for concentrations from 10 wt% to 80 wt% amphiphile, in the temperature range 25 °C to >100 °C. Lyotropic liquid crystalline phases (hexagonal, cubic and lamellar) were formed at high surfactant concentrations (typically >50 wt%), whereas at thermal stability of the phases formed by these surfactants persisted to temperatures above 100 °C. The phase behaviour of amphiphile-PIL systems was interpreted by considering the PIL cohesive energy, liquid nanoscale order, polarity and ionicity. For comparison the phase behaviour of the four amphiphiles was also studied in water.

Elimination of liquid discharge to the environment from the TA-50 Radioactive Liquid Waste Treatment Facility

International Nuclear Information System (INIS)

Moss, D.; Williams, N.; Hall, D.; Hargis, K.; Saladen, M.; Sanders, M.; Voit, S.; Worland, P.; Yarbro, S.

1998-06-01

Alternatives were evaluated for management of treated radioactive liquid waste from the radioactive liquid waste treatment facility (RLWTF) at Los Alamos National Laboratory. The alternatives included continued discharge into Mortandad Canyon, diversion to the sanitary wastewater treatment facility and discharge of its effluent to Sandia Canyon or Canada del Buey, and zero liquid discharge. Implementation of a zero liquid discharge system is recommended in addition to two phases of upgrades currently under way. Three additional phases of upgrades to the present radioactive liquid waste system are proposed to accomplish zero liquid discharge. The first phase involves minimization of liquid waste generation, along with improved characterization and monitoring of the remaining liquid waste. The second phase removes dissolved salts from the reverse osmosis concentrate stream to yield a higher effluent quality. In the final phase, the high-quality effluent is reused for industrial purposes within the Laboratory or evaporated. Completion of these three phases will result in zero discharge of treated radioactive liquid wastewater from the RLWTF

Elimination of liquid discharge to the environment from the TA-50 Radioactive Liquid Waste Treatment Facility

Energy Technology Data Exchange (ETDEWEB)

Moss, D.; Williams, N.; Hall, D.; Hargis, K.; Saladen, M.; Sanders, M.; Voit, S.; Worland, P.; Yarbro, S.

1998-06-01

Alternatives were evaluated for management of treated radioactive liquid waste from the radioactive liquid waste treatment facility (RLWTF) at Los Alamos National Laboratory. The alternatives included continued discharge into Mortandad Canyon, diversion to the sanitary wastewater treatment facility and discharge of its effluent to Sandia Canyon or Canada del Buey, and zero liquid discharge. Implementation of a zero liquid discharge system is recommended in addition to two phases of upgrades currently under way. Three additional phases of upgrades to the present radioactive liquid waste system are proposed to accomplish zero liquid discharge. The first phase involves minimization of liquid waste generation, along with improved characterization and monitoring of the remaining liquid waste. The second phase removes dissolved salts from the reverse osmosis concentrate stream to yield a higher effluent quality. In the final phase, the high-quality effluent is reused for industrial purposes within the Laboratory or evaporated. Completion of these three phases will result in zero discharge of treated radioactive liquid wastewater from the RLWTF.

Stainless austenitic steels strengthened due to reversible phase transformations and by ageing

International Nuclear Information System (INIS)

Sagaradze, V.V.; Kositsyna, I.I.; Ozhiganov, A.V.

1981-01-01

The effect of the reversible phase transformations, consisting in the conduction of the direct and reverse martensite transformations and aging, during which the intermetallide γ'-phase of the composition Ni 3 Ti is formed, on the streng-thening of alloys in the Fe-Cr-Ni-Ti system is considered. Stainless austenitic steels Kh12N12T3 and Kh12N14T3, which acquire high mechanical properties: σsub(0.2)=685-785 MPa, σsub(B)=1275 MPa, delta >= 20%, as a result of reversible phase transformations and aging, are suggested. After the reversible phase transformations and ageing the steels possess a high resistance to γ-α-transformation during cold treatment [ru

Open loop, auto reversing liquid nitrogen circulation thermal system for thermo vacuum chamber

International Nuclear Information System (INIS)

Naidu, M C A; Nolakha, Dinesh; Saharkar, B S; Kavani, K M; Patel, D R

2012-01-01

In a thermo vacuum chamber, attaining and controlling low and high temperatures (-100 Deg. C to +120 Deg. C) is a very important task. This paper describes the development of 'Open loop, auto reversing liquid nitrogen based thermal system'. System specifications, features, open loop auto reversing system, liquid nitrogen flow paths etc. are discussed in this paper. This thermal system consists of solenoid operated cryogenic valves, double embossed thermal plate (shroud), heating elements, temperature sensors and PLC. Bulky items like blowers, heating chambers, liquid nitrogen injection chambers, huge pipe lines and valves were not used. This entire thermal system is very simple to operate and PLC based, fully auto system with auto tuned to given set temperatures. This system requires a very nominal amount of liquid nitrogen (approx. 80 liters / hour) while conducting thermo vacuum tests. This system was integrated to 1.2m dia thermo vacuum chamber, as a part of its augmentation, to conduct extreme temperature cycling tests on passive antenna reflectors of satellites.

Temperature induced reversible polymorphic phase transformations in a bis-hydrazone compound

Science.gov (United States)

Jayant, Vikrant; Das, Dinabandhu

2018-03-01

Two reversible polymorphic phase transformation of 2,3-butanedione, 2,3- bis[4,4‧-bis(diethylamino)benzophenone hydrazone] (DEBH) have been identified in DSC experiment. Topotactic phase transformation of three polymorphs has been observed in variable temperature Single Crystal X-ray Diffraction experiment. The reversible phase transformation of bulk material has been confirmed by Powder X-ray diffraction study.

Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements.

Science.gov (United States)

Li, Jing; Roh, Si Hun; Shaodong, Jia; Hong, Ji Yeon; Lee, Dong-Kyu; Shin, Byong-Kyu; Park, Jeong Hill; Lee, Jeongmi; Kwon, Sung Won

2017-08-01

A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Martensite shear phase reversion-induced nanograined/ultrafine-grained Fe-16Cr-10Ni alloy: The effect of interstitial alloying elements and degree of austenite stability on phase reversion

Energy Technology Data Exchange (ETDEWEB)

Misra, R.D.K., E-mail: dmisra@louisiana.edu [Center for Structural and Functional Materials, University of Louisiana at Lafayette, Madison Hall Room 217, P.O. Box 44130, Lafayette, LA 70504-1430 (United States); Zhang, Z.; Venkatasurya, P.K.C. [Center for Structural and Functional Materials, University of Louisiana at Lafayette, Madison Hall Room 217, P.O. Box 44130, Lafayette, LA 70504-1430 (United States); Somani, M.C.; Karjalainen, L.P. [Department of Mechanical Engineering, University of Oulu, P.O. Box 4200, Oulu 90014 (Finland)

2010-11-15

Research highlights: {yields} Development of a novel process involving phase-reversion annealing process. {yields} Austensite stability strongly influences development of nanograined structure. {yields} Interstitial elements influence microstructural evolution during annealing. - Abstract: We describe here an electron microscopy study of microstructural evolution associated with martensitic shear phase reversion-induced nanograined/ultrafine-grained (NG/UFG) structure in an experimental Fe-16Cr-10Ni alloy with very low interstitial content. The primary objective is to understand and obtain fundamental insights on the influence of degree of austenite stability (Fe-16Cr-10Ni, 301LN, and 301 have different austenite stability index) and interstitial elements (carbon and nitrogen) in terms of phase reversion process, microstructural evolution during reversion annealing, and temperature-time annealing sequence. A relative comparison of Fe-16Cr-10Ni alloy with 301LN and 301 austenitic stainless steels indicated that phase reversion in Fe-16Cr-10Ni occurred by shear mechanism, which is similar to that observed for 301, but is different from the diffusional mechanism in 301LN steel. While the phase reversion in the experimental Fe-16Cr-10Ni alloy and 301 austenitic stainless steel occurred by shear mechanism, there were fundamental differences between these two alloys. The reversed strain-free austenite grains in Fe-16Cr-10Ni alloy were characterized by nearly same crystallographic orientation, where as in 301 steel there was evidence of break-up of martensite laths during reversion annealing resulting in several regions of misoriented austenite grains in 301 steel. Furthermore, a higher phase reversion annealing temperature range (800-900 deg. C) was required to obtain a fully NG/UFG structure of grain size 200-600 nm. The difference in the phase reversion and the temperature-time sequence in the three stages is explained in terms of Gibbs free energy change that

Studies on radioactive liquid waste treatment by reverse osmosis

International Nuclear Information System (INIS)

Koyama, Akio; Shimoura, Kazukuni; Tsutsui, Tenson

1982-01-01

Reverse osmosis is a simple process and has relatively high decontamination factor comparing to other processes used for the treatment of radioactive liquid waste. Furthermore the quantity of secondary waste of this process is small. In this study, test solution containing nine elements such as cesium, strontium, cobalt etc. in chloride forms are treated by reverse osmosis. Permeate rate decreases as the increase of osmotic pressure of feed solution and is expressed by linear equation. Decontamination factor of cations of univalency is more than ten, and about one tenth of that of bivalency. Decontamination factors of all the elements used in this experiment are approximately estimated using the solution-diffusion model. (author)

Elution behavior of N-heterocyclic derivatives of mixed ruthenium(II)-sulfoxide complexes in reversed-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Toma, H.E.; Silva, D.O.

1991-01-01

The elution behaviour of a series of dichlorobis-(dimethylsulfoxide)bis(N-heterocyclic) ruthenium(II) complexes has been investigated using reversed-phase HPLC. Similar trends as those displayed by the free N-heterocyclic bases have been observed for the complexes, essentially reflecting the hydrophobic properties of the aromatic ligands. (orig.)

Initiation of geyser during the resettlement of cryogenic liquid under impulsive reverse gravity acceleration in microgravity environment

Science.gov (United States)

Hung, R. J.; Shyu, K. L.

1991-01-01

The requirement to settle or to position liquid fluid over the outlet end of spacecraft propellant tank prior to main engine restart poses a microgravity fluid behavior problem. Resettlement or reorientation of liquid propellant can be accomplished by providing optimal acceleration to the spacecraft such that the propellant is reoriented over the tank outlet without any vapor entrainment, any excessive geysering, or any other undesirable fluid motion for the space fluid management under microgravity environment. The purpose of present study is to investigate most efficient technique for propellant resettling through the minimization of propellant usage and weight penalties. Comparison between the constant reverse gravity acceleration and impulsive reverse gravity acceleration to be used for the activation of propellant resettlement, it shows that impulsive reverse gravity thrust is superior to constant reverse gravity thrust for liquid reorientation in a reduced gravity environment.

Analyses of Indole Compounds in Sugar Cane (Saccharum officinarum L. Juice by High Performance Liquid Chromatography and Liquid Chromatography-Mass Spectrometry after Solid-Phase Extraction

Directory of Open Access Journals (Sweden)

Jean Wan Hong Yong

2017-03-01

Full Text Available Simultaneous quantitative analysis of 10 indole compounds, including indole-3-acetic acid (IAA, one of the most important naturally occurring auxins and some of its metabolites, by high performance liquid chromatography (HPLC and liquid chromatography-mass spectrometry (LC-MS after solid-phase extraction (SPE was reported for the first time. The analysis was carried out using a reverse phase HPLC gradient elution, with an aqueous mobile phase (containing 0.1% formic acid modified by methanol. Furthermore, a novel SPE procedure was developed for the pre-concentration and purification of indole compounds using C18 SPE cartridges. The combination of SPE, HPLC, and LC-MS was applied to screen for the indole compounds present in sugar cane (Saccharum officinarum L. juice, a refreshing beverage with various health benefits. Finally, four indole compounds were successfully detected and quantified in sugar cane juice by HPLC, which were further unequivocally confirmed by LC-MS/MS experiments operating in the multiple reaction monitoring (MRM mode.

Acidic ionic liquids for n-alkane isomerization in a liquid-liquid or slurry-phase reaction mode

Energy Technology Data Exchange (ETDEWEB)

Meyer, C.; Hager, V.; Geburtig, D.; Kohr, C.; Wasserscheid, P. [Erlangen-Nuernberg Univ. (Germany). Lehrstuhl fuer Chemische Reaktionstechnik; Haumann, M. [Chemical Reaction Engineering, FAU Busan Campus, Korea (Korea, Republic of)

2011-07-01

Highly acidic ionic liquid (IL) catalysts offer the opportunity to convert n-alkanes at very low reaction temperatures. The results of IL catalyzed isomerization and cracking reactions of pure n-octane are presented. Influence of IL composition, [C{sub 4}C{sub 1}Im]Cl / AlCl{sub 3} / H{sub 2}SO{sub 4} and [C{sub 4}C{sub 1}Im]Cl / AlCl{sub 3} / 1-chlorooctane, on catalyst activity and selectivities to branched alkanes was investigated. Acidic chloroaluminate IL catalysts form liquid-liquid biphasic systems with unpolar organic product mixtures. Thus, recycling of the acidic IL is enabled by simple phase separation in the liquid-liquid biphasic reaction mode or the IL can be immobilized on an inorganic support with a large specific surface area. These supported ionic liquid phase (SILP) catalysts offer the advantage to get a macroscopically heterogeneous system while still preserving all benefits of the homogeneous catalyst which can be used for the slurry-phase n-alkane isomerization. The interaction of the solid support and acidic IL influences strongly the catalytic activity. (orig.)

Preliminary investigation of liquid phase sintering in ferrous systems

International Nuclear Information System (INIS)

Klein, J.

1975-04-01

Liquid phase sintering was utilized to achieve, by a simple compaction and sintering procedure involving short times and moderate temperatures, a virtually full dense high carbon Fe:C alloy and high boron Fe:B alloy. Parameters such as powder characteristics and mixing, compacting pressure, heating program and the liquid phase fraction were found to influence the sintered density. The response of the Fe:C alloy to a heat treatment is reported along with preliminary experiments in the iron base ternary system Fe:W:C. Residual porosities observed in microstructures of certain liquid phase sintered compacts were accounted for by a proposed capillary flow of the liquid phase and a local densification competing against an overall densification. Some general recommendations are made for liquid phase sintering of powder aggregates. 15 fig., 7 tables

Reclaimable Thermally Reversible Polymers for AM Feedstock, Phase II

Data.gov (United States)

National Aeronautics and Space Administration — CRG proposes to continue efforts from the 2016 NASA SBIR Phase I topic H5.04 Reclaimable Thermally Reversible Polymers for AM Feedstock. In Phase II, CRG will refine...

Simultaneous determination of caffeine, theophylline and theobromine in human plasma by on-line solid-phase extraction coupled to reversed-phase chromatography.

Science.gov (United States)

Emara, Samy

2004-10-01

A reversed-phase liquid chromatographic column switching system was described for the determination of caffeine (CF), theophylline (TH) and theobromine (TB) in human plasma with a direct injection procedure. A short protein-coated mu Bondapak CN silica pre-column (20 x 3 mm, i.d.) was used for enrichment of the drugs and clean up from weakly retained plasma components using phosphate buffer saline pH 7.4. After washing step, the retained drugs were flushed into a reversed-phase column (5 microm TSK gel ODS-80 TM, 150 x 4.6 mm i.d.) with a mobile phase of methanol-0.01 M phosphate buffer, pH 3.5 (30:70, v/v) for the final separation. The eluent was monitored with a UV detector at 275 nm. The resulting chromatograms showed no interference from endogenous plasma components. A linear relationship between the concentration of drug and peak height was confirmed in the range of 0.5-20 microg/mL for all drugs. High extraction recoveries from plasma ranging from 96.12 to 100.32% were achieved. Validation of the method was examined performing intra- and inter-day accuracy and precision and was found to be satisfactory. The coefficients of variation of the three drugs were less than 3% for intra-day and less than 4% for inter-day run assays.

Development and validation of reversed-phase HPLC gradient method for the estimation of efavirenz in plasma.

Directory of Open Access Journals (Sweden)

Shweta Gupta

Full Text Available Efavirenz is an anti-viral agent of non-nucleoside reverse transcriptase inhibitor category used as a part of highly active retroviral therapy for the treatment of infections of human immune deficiency virus type-1. A simple, sensitive and rapid reversed-phase high performance liquid chromatographic gradient method was developed and validated for the determination of efavirenz in plasma. The method was developed with high performance liquid chromatography using Waters X-Terra Shield, RP18 50 x 4.6 mm, 3.5 μm column and a mobile phase consisting of phosphate buffer pH 3.5 and Acetonitrile. The elute was monitored with the UV-Visible detector at 260 nm with a flow rate of 1.5 mL/min. Tenofovir disoproxil fumarate was used as internal standard. The method was validated for linearity, precision, accuracy, specificity, robustness and data obtained were statistically analyzed. Calibration curve was found to be linear over the concentration range of 1-300 μg/mL. The retention times of efavirenz and tenofovir disoproxil fumarate (internal standard were 5.941 min and 4.356 min respectively. The regression coefficient value was found to be 0.999. The limit of detection and the limit of quantification obtained were 0.03 and 0.1 μg/mL respectively. The developed HPLC method can be useful for quantitative pharmacokinetic parameters determination of efavirenz in plasma.

Removal of radionuclides from liquid streams by reverse osmosis

International Nuclear Information System (INIS)

Deshmukh, U.A.; Ramachandhran, V.; Misra, B.M.

1987-01-01

Separation of radionuclides in trace concentrations by cellulose acetate membranes has been under investigation in this laboratory, and the behaviour of some important radionuclides such as 137 Cs and 90 Sr under reverse osmosis has been reported earlier. The present work deals with a few other typical radionuclides such as 60 Co, 103 Ru and 131 I which are not fully amenable to conventional methods for their removal. Separation of these radionuclides from liquid streams by the reverse osmosis process was studied using a small reverse osmosis test cell. Various parameters like membrane porosity, applied pressure and feed activity levels were investigated. Cellulose acetate membranes offer reasonable separation of 60 Co, 103 Ru and 131 I radionuclides, indicating the potential of reverse osmosis for treatment of effluents containing these radioisotopes. The percent separation is found to be in the order of Co > Ru > I. The percent radioactive separation improves with increases in feed activity. The performance data are explained in terms of solution-diffusion mechanism. It appears that the separation of radionuclides is not governed by diffusion alone, but by the interaction of solutes with the membranes. (author)

Selective gas absorption by ionic liquids

DEFF Research Database (Denmark)

Shunmugavel, Saravanamurugan; Kegnæs, Søren; Due-Hansen, Johannes

2010-01-01

Reversible absorption performance for the flue gas components CO 2, NO and SO2 has been tested for several different ionic liquids (ILs) at different temperatures and flue gas compositions. Furthermore, different porous, high surface area carriers have been applied as supports for the ionic liquids...... to obtain Supported Ionic Liquid-Phase (SILP) absorber materials. The use of solid SILP absorbers with selected ILs were found to significantly improve the absorption capacity and sorption dynamics at low flue gas concentration, thus making the applicability of ILs viable in technical, continuous flow...... processes for flue gas cleaning. The results show that CO 2, NO and SO2 can be reversible and selective absorbed using different ILs and that Supported Ionic Liquid-Phase (SILP) absorbers are promising materials for industrial flue gas cleaning. Absorption/desorption dynamics can be tuned by temperatures...

Evaluation of chromatographic conditions in reversed phase liquid chromatography-mass spectrometry systems for fingerprinting of polar and amphiphilic plant metabolites

DEFF Research Database (Denmark)

Nielsen, Nikoline Juul; Tomasi, Giorgio; Christensen, Jan H.

2016-01-01

Metabolic fingerprinting is a relatively young scientific discipline requiring robust, yet flexible and fit-for-purpose analytical methods. Here, we introduce a simple approach to select reversed phase LC systems with electrospray MS detection for fingerprinting of polar and amphiphilic plant met...

Predicting glass-to-glass and liquid-to-liquid phase transitions in supercooled water using classical nucleation theory

Science.gov (United States)

Tournier, Robert F.

2018-01-01

Glass-to-glass and liquid-to-liquid phase transitions are observed in bulk and confined water, with or without applied pressure. They result from the competition of two liquid phases separated by an enthalpy difference depending on temperature. The classical nucleation equation of these phases is completed by this quantity existing at all temperatures, a pressure contribution, and an enthalpy excess. This equation leads to two homogeneous nucleation temperatures in each liquid phase; the first one (Tn- below Tm) being the formation temperature of an "ordered" liquid phase and the second one corresponding to the overheating temperature (Tn+ above Tm). Thermodynamic properties, double glass transition temperatures, sharp enthalpy and volume changes are predicted in agreement with experimental results. The first-order transition line at TLL = 0.833 × Tm between fragile and strong liquids joins two critical points. Glass phase above Tg becomes "ordered" liquid phase disappearing at TLL at low pressure and at Tn+ = 1.302 × Tm at high pressure.

Graphene/phase change material nanocomposites: light-driven, reversible electrical resistivity regulation via form-stable phase transitions.

Science.gov (United States)

Wang, Yunming; Mi, Hongyi; Zheng, Qifeng; Ma, Zhenqiang; Gong, Shaoqin

2015-02-04

Innovative photoresponsive materials are needed to address the complexity of optical control systems. Here, we report a new type of photoresponsive nanomaterial composed of graphene and a form-stable phase change material (PCM) that exhibited a 3 orders of magnitude change in electrical resistivity upon light illumination while retaining its overall original solid form at the macroscopic level. This dramatic change in electrical resistivity also occurred reversibly through the on/off control of light illumination. This was attributed to the reversible phase transition (i.e., melting/recrystallization) behavior of the microscopic crystalline domains present in the form-stable PCM. The reversible phase transition observed in the graphene/PCM nanocomposite was induced by a reversible temperature change through the on/off control of light illumination because graphene can effectively absorb light energy and convert it to thermal energy. In addition, this graphene/PCM nanocomposite also possessed excellent mechanical properties. Such photoresponsive materials have many potential applications, including flexible electronics.

Supported Ionic Liquid Phase (SILP) catalysis

DEFF Research Database (Denmark)

Riisager, Anders; Fehrmann, Rasmus; Haumann, Marco

2006-01-01

Applications of ionic liquids to replace conventional solvents in homogeneous transition-metal catalysis have increased significantly during the last decade. Biphasic ionic liquid/organic liquid systems offer advantages with regard to product separation, catalyst stability, and recycling...... but utilise in the case of fast chemical reactions only a small amount of expensive ionic liquid and catalyst. The novel Supported Ionic Liquid Phase (SILP) catalysis concept overcomes these drawbacks and allows the use of fixed-bed reactors for continuous reactions. In this Microreview the SILP catalysis...

Reversible Rigidity Control Using Low Melting Temperature Alloys

Science.gov (United States)

Shan, Wanliang; Lu, Tong; Majidi, Carmel

2013-03-01

Inspired by nature, materials able to achieve rapid rigidity changes have important applications for human body protection in military and many other areas. This talk presents the fabrication and design of soft-matter technologies that exhibit rapid reversible rigidity control. Fabricated with a masked deposition technique, the soft-matter composite contains liquid-phase and phase-changing metal alloys embedded in a soft and highly stretchable elastomer. The composite material can reversibly change its rigidity by three orders of magnitude and sustain large deformation.

A Thermal Degradation (Thermolysis) Study of Rotenone Extracted from Derris elliptica Roots Using Reverse-Phase High Performance Liquid Chromatography (RP-HPLC)

International Nuclear Information System (INIS)

Saiful Irwan Zubairi; Mohamad Roji Sarmidi; Ramlan Abdul Aziz

2015-01-01

Bio-pesticides are becoming increasingly important as pest management tools in various cropping systems in the tropics essentially to remedy problems associated with the indiscriminate use of hard and non-environmental friendly inorganic pesticide. In these past few decades, many bio-pesticidal products, both microbial-based (bacteria, fungi, microsprodia, entomopathogenic nematodes and viruses) and plant-based botanicals (rotenone and azadiracthin) have been studied for their use against insect pests in the tropics. In this study, the effects of the concentration process with respect to the yield of rotenone (mg) and its concentration (mg/mL) are presented extensively. The raw plants were collected from Kota Johor Lama, Johor and sorted to obtain the roots and stems. Only the roots and stems were utilized as raw materials of the extraction process. The rotenone from roots and stems was extracted using the normal soaking extraction (NSE) at 28 to 30 degree Celsius with 95 % (v/v) of acetone as a solvent and the solvent-to-solid ratio of 10 mL/ g. The extraction was carried out for 24 h. Next, the liquid crude extract was concentrated using the rotary evaporator at 50 degree Celsius and 80 mbar of vacuum pressure to remove approximately 90 % of solvent. The fractions of the liquid crude extract were collected (15 min/ mL/ fraction), diluted (1/100 with acetone) and cleaned up (to remove any fine debris) prior to determination of rotenone content (mg) and concentration (mg/mL) by using the reverse-phase high performance liquid chromatography (RP-HPLC). Finally, the results showed that there was a significant effect of thermal degradation or dissipation of rotenone content at higher operating temperature (greater than 40 degree Celsius) with a rapid rotenone reduction for the first 15 min of exposure. The possibilities for better exploitation and identification of the effective operating parameters based on the above mentioned results will be perhaps discussed in the

[Simultaneous determination of principal components and related substances of raw material drug of ammonium glycyrrhizinate by reversed-phase high performance liquid chromatography].

Science.gov (United States)

Zhao, Yanyan; Liu, Liyan; Han, Yuanyuan; Li, Yueqiu; Wang, Yan; Shi, Minjian

2013-09-01

An analytical method for the simultaneous determination of 18alpha-glycyrrhizic acid, 18beta-glycyrrhizinic acid, related substances A and B and drug quality standard by reversed-phase high performance liquid chromatography (RP-HPLC) was established. The assay was carried out on a Durashell-C18 column (250 mm x 4.6 mm, 5 microm) with 10 mmol/L ammonium perchlorate (the pH value was adjusted to 8.20 with ammonia)-methanol (48:52, v/v) as mobile phase at a flow rate of 0.80 mL/min, and the detection wavelength was set at 254 nm. The column temperature was 50 degrees C and the injection volume was 10 microL. Under the separation conditions, the calibration curves of the analytes showed good linearities within the mass concentrations of 0.50 -100 mg/L (r > 0.999 9). The detection limits for 18alpha-glycyrrhizic acid, 18beta-glycyrrhizinic acid, related substances A and B were 0.15, 0.10, 0.10, 0.15 mg/L, respectively. The average recoveries were between 97.32% and 99.33% (n = 3) with the relative standard deviations (RSDs) between 0.05% and 1.06%. The method is sensitive, reproducible, and the results are accurate and reliable. The method can be used for the determination of principal components and related substances of ammonium glycyrrhizinate for the quality control of raw material drug of ammonium glycyrrhizinate.

Development and validation of a dissolution test with reversed-phase high performance liquid chromatographic analysis for Candesartan cilexetil in tablet dosage forms

Directory of Open Access Journals (Sweden)

Vairappan Kamalakkannan

2016-09-01

Full Text Available A simple, rapid, selective and reproducible reversed-phase high performance liquid chromatographic (RP-HPLC method has been developed and validated for the estimation of release of Candesartan cilexetil (CC in tablets. Analysis was performed on an Agilent, Zorbax C8 column (150mm × 4.6mm, 5μm with the mobile phase consisting of phosphate buffer (pH2.5–acetonitrile (15:85, v/v at a flow rate of 1.0mL/min. UV detection was performed at 215nm and the retention time for CC was 2.2. The calibration curve was linear (correlation coefficient = 1.000 in the selected range of analyte. The optimized dissolution conditions include the USP apparatus 2 at a paddle rotation rate of 50rpm and 900mL of phosphate buffer (pH7.2 with 0.03% of polysorbate 80 as dissolution medium, at 37.0 ± 0.5°C. The method was validated for precision, linearity, specificity, accuracy, limit of quantitation and ruggedness. The system suitability parameters, such as theoretical plate, tailing factor and relative standard deviation (RSD between six standard replicates were well within the limits. The stability result shows that the drug is stable in the prescribed dissolution medium. Three different batches (A, B and C of the formulation containing 8mg of Candesartan cilexetil was performed with the developed method and the results showed no significant differences among the batches.

Solid-phase extraction and high-performance liquid chromatographic separation of pigments of red wines.

Science.gov (United States)

Csiktusnádi Kiss, G A; Forgács, E; Cserháti, T; Candeias, M; Vilas-Boas, L; Bronze, R; Spranger, I

2000-08-11

The adsorption and desorption capacities of 11 different solid-phase extraction sorbents were tested for the preconcenration of pigments of various Hungarian red wines. The concentrates were evaluated by multiwavelengh spectrophotometry combined with a spectral mapping technique (SPM) and by reversed-phase high-performance liquid chromatography. The highest (10-fold) concentration of pigments was achieved on octadecylsilica sorbent. It can be used five times without losing adsorption and desorption characteristics. SPM indicated that multiwavelength spectrophotometry can be employed for the differentiation of red wines. Comparison of the chromatograms of pigments with and without preconcentration showed that preconcentration makes possible the separation and detection of pigments present in low concentration in red wines.

Two-dimensional high-performance thin-layer chromatography of tryptic bovine albumin digest using normal- and reverse-phase systems with silanized silica stationary phase.

Science.gov (United States)

Gwarda, Radosław Łukasz; Dzido, Tadeusz Henryk

2013-10-18

Among many advantages of planar techniques, two-dimensional (2D) separation seems to be the most important for analysis of complex samples. Here we present quick, simple and efficient two-dimensional high-performance thin-layer chromatography (2D HPTLC) of bovine albumin digest using commercial HPTLC RP-18W plates (silica based stationary phase with chemically bonded octadecyl ligands of coverage density 0.5μmol/m(2) from Merck, Darmstadt). We show, that at low or high concentration of water in the mobile phase comprised methanol and some additives the chromatographic systems with the plates mentioned demonstrate normal- or reversed-phase liquid chromatography properties, respectively, for separation of peptides obtained. These two systems show quite different separation selectivity and their combination into 2D HPTLC process provides excellent separation of peptides of the bovine albumin digest. Copyright © 2013 Elsevier B.V. All rights reserved.

Pharmaceutical Perspective on Opalescence and Liquid-Liquid Phase Separation in Protein Solutions.

Science.gov (United States)

Raut, Ashlesha S; Kalonia, Devendra S

2016-05-02

Opalescence in protein solutions reduces aesthetic appeal of a formulation and can be an indicator of the presence of aggregates or precursor to phase separation in solution signifying reduced product stability. Liquid-liquid phase separation of a protein solution into a protein-rich and a protein-poor phase has been well-documented for globular proteins and recently observed for monoclonal antibody solutions, resulting in physical instability of the formulation. The present review discusses opalescence and liquid-liquid phase separation (LLPS) for therapeutic protein formulations. A brief discussion on theoretical concepts based on thermodynamics, kinetics, and light scattering is presented. This review also discusses theoretical concepts behind intense light scattering in the vicinity of the critical point termed as "critical opalescence". Both opalescence and LLPS are affected by the formulation factors including pH, ionic strength, protein concentration, temperature, and excipients. Literature reports for the effect of these formulation factors on attractive protein-protein interactions in solution as assessed by the second virial coefficient (B2) and the cloud-point temperature (Tcloud) measurements are also presented. The review also highlights pharmaceutical implications of LLPS in protein solutions.

Liquid-liquid phase separation in internally mixed magnesium sulfate/glutaric acid particles

Science.gov (United States)

Wu, Feng-Min; Wang, Xiao-Wei; Jing, Bo; Zhang, Yun-Hong; Ge, Mao-Fa

2018-04-01

The confocal Raman microscopy is utilized to investigate the liquid-liquid phase separation (LLPS) of mixed magnesium sulfate/glutaric acid (MgSO4/GA) droplets deposited on a hydrophobic polytetrafluoroethylene (PTFE) substrate and a hydrophilic quartz substrate. Raman spectra collected from different regions of the mixed droplets provide detailed information of component distributions for MgSO4 and GA. During the dehydration process, the MgSO4/GA mixed particles show the initial liquid-liquid phase separation between 85% and 80% relative humidity (RH) on both the hydrophobic and hydrophilic substrates. For the droplets deposited on the two substrates, the inner phase of droplets is dominated by aqueous MgSO4, which is surrounded by a rich GA organic layer due to the surface tension effects. In addition, the crystallization of GA could be observed in the organic aqueous phase while it is inhibited in the inner MgSO4 phase due to the effects of gel formation of MgSO4 at low RH. The Raman spectra reveal that with decreasing RH the morphology of the mixed droplet evolves from a uniform droplet to the structure of LLPS with the GA crystallizing in the outer layer and MgSO4 gel formed in the inner phase. These findings contribute to the further understanding of the role of interactions between inorganic salts and organic acids on the morphological evolution and environmental effects of atmospheric aerosols under ambient RH conditions.

Separation of uranium from aqueous solutions using calix[6]arenes in liquid-liquid extraction as well as solid phase extraction

International Nuclear Information System (INIS)

Schmeide, K.; Geipel, G.; Bernhard, G.

2004-11-01

The suitability of different calyx[n] arene types for uranyl extraction from liquid solutions was examined by means of liquid-liquid extraction using aqueous phases and organic solvents of varying compositions. It was found that COOH-derivatised calyx[6] arenes have good extraction properties and can even be used in the acid pH range. The use of calixarene-modified fleeces for the separation of uranyl from aqueous phases was examined in batch experiments with pH and uranyl concentration as variables and in the presence or absence of competing ions. The results showed that calixarene-modified fleeces can be used for uranium separation starting from pH 4. At pH 5, up to a maximum of 7.6 x 10 -7 mol uranium can be bound per 1 g of calixarene-modified fleece. The separation of uranyl from synthetic pit waters was examined as a means of testing the separation capacity of calixarene-modified fleeces in environmentally sensitive waters. Studies on the reversibility of uranium bonding to calixarene-treated polyester fleeces have shown that under environmentally realistic conditions (neutral pH range) the uranium is firmly bound to the calixarene-modified fleeces and cannot be mobilised. By contrast, in acidic environments calixarene-modified fleeces are capable of near-complete regeneration. Such regenerated textile filter materials can then be used for further uranium separation cycles [de

PURIFICATION OF Cd-BINDING PROTEIN FROM MAIZE ROOTS BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

Institute of Scientific and Technical Information of China (English)

何笃修; 罗建沅; 全胜

1991-01-01

An efficient procedure of purification of Cd-binding protein in roots of maize has been established. Young seedlings of maize were exposed to a medium containing CdCl2 to induce the production of Cd-binding protein in their roots. The protein was purified after heat treatment by ion-exchange chromatography and reverse-phase HPLC. The resulting protein was identified as a purified product by N-terminal amino acid with the dansyl method. Its molecular weight was 3200 dalton, the cysteine content was 29.5%, about 3 Cd atoms were bound to one molecule of the protein and the Cd : cystine ratio was 1 : 2.3. According to its character, this protein could be a kind of plant metallothionein-like protein.

Mixed-mode reversed phase/positively charged repulsion chromatography for intact protein separation.

Science.gov (United States)

Ding, Ling; Guo, Zhimou; Hu, Zhuo; Liang, Xinmiao

2017-05-10

A mixed-mode reversed phase/positively charged repulsion stationary phase C8PN composed of octyl and amino group has been developed for separation of intact protein. Before the separation of proteins, a set of probe compounds were employed to evaluate the chromatographic properties of C8PN, demonstrating typical reversed phase/positively charged repulsion interaction on this stationary phase as estimated. Then the new C8PN stationary phase was used to separate a standard protein mixture on the reversed phase mode. Compared with a commercial C4 stationary phase, it showed different selectivity for some proteins. In order to better understand the properties of C8PN, the effect of acetonitrile content was investigated based on retention equation. Higher values of the equation parameters on C8PN demonstrated that the protein retentions were more sensitive to the change of acetonitrile content. Besides, the influences of buffer salt additives on the protein retentions were also studied. The retention factors of the proteins got larger with the increase of buffer salt concentration, which confirmed the positively charged repulsion interaction on the column. Finally, the C8PN was further applied to separate oxidized- and reduced- forms of Recombinant Human Growth Hormone. Our study indicated the advantages and application potential of mixed-mode reversed phase/positively charged repulsion stationary phase for intact protein separation. Copyright © 2017 Elsevier B.V. All rights reserved.

Distinction of synthetic dl-α-tocopherol from natural vitamin E (d-α-tocopherol) by reversed-phase liquid chromatography. Enhanced selectivity of a polymeric C18 stationary phase at low temperature and/or at high pressure.

Science.gov (United States)

Yui, Yuko; Miyazaki, Shota; Ma, Yan; Ohira, Masayoshi; Fiehn, Oliver; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

2016-06-10

Separation of diastereomers of dl-α-tocopherol was studied by reversed-phase liquid chromatography using three types of stationary phases, polymeric ODS, polymeric C30, and monomeric ODS. Polymeric ODS stationary phase (Inertsil ODS-P, 3mmID, 20cm) was effective for the separation of the isomers created by the presence of three chiral centers on the alkyl chain of synthetic dl-α-tocopherol. Considerable improvement of the separation of isomers was observed on ODS-P phase at high pressure and at low temperature. Complete separation of four pairs of diastereomers was achieved at 12.0°C, 536bar, while three peaks were observed when the separation was carried out either at 12.0°C at low pressure or at 20°C at 488bar. Higher temperature (30.0°C) with the ODS-P phase resulted in only partial separation of the diastereomers even at high pressure. Only slight resolution was observed for the mixture of diastereomers with the C30 stationary phase (Inertsil C30) at 12.0°C and 441bar, although the stationary phase afforded greater resolution for β- and γ-tocopherol than ODS-P. A monomeric C18 stationary phase did not show any separation at 12.0°C and 463bar. The results suggest that the binding site of the polymeric ODS-P phase is selective for flexible alkyl chains that provided the longest retention for the natural form, (R,R,R) form, and the enantiomer, (S,S,S) form, of dl-α-tocopherol. Copyright © 2016. Published by Elsevier B.V.

Industrial aspects of gas-liquid two-phase flow

International Nuclear Information System (INIS)

Hewitt, G.F.

1977-01-01

The lecture begins by reviewing the various types of plant in which two phase flow occurs. Specifically, boiling plant, condensing plant and pipelines are reviewed, and the various two phase flow problems occurring in them are described. Of course, many other kinds of chemical engineering plant involve two phase flow, but are somewhat outside the scope of this lecture. This would include distillation columns, vapor-liquid separators, absorption towers etc. Other areas of industrial two phase flow which have been omitted for space reasons from this lecture are those concerned with gas/solids, liquid/solid and liquid/liquid flows. There then follows a description of some of the two phase flow processes which are relevant in industrial equipment and where special problems occur. The topics chosen are as follows: (1) pressure drop; (2) horizontal tubes - separation effects non-uniformites in heat transfer coefficient, effect of bends on dryout; (3) multicomponent mixtures - effects in pool boiling, mass transfer effects in condensation and Marangoni effects; (4) flow distribution - manifold problems in single phase flow, separation effects at a single T-junction in two phase flow and distribution in manifolds in two phase flow; (5) instability - oscillatory instability, special forms of instability in cryogenic systems; (6) nucleate boiling - effect of variability of surface, unresolved problems in forced convective nucleate boiling; and (7) shell side flows - flow patterns, cross flow boiling, condensation in cross flow

A copper-mediated reverse aromatic Finkelstein reaction in ionic liquid

Directory of Open Access Journals (Sweden)

Anh T.H. Nguyen

2018-03-01

Full Text Available We have developed a general method for reverse aromatic Finkelstein reactions. Good reaction yields were obtained when aryl iodides or aryl bromides were treated with copper halide salts as promoters in a 1-butyl-3-methylimidazolium bromide ([BMIM]Br ionic liquid (IL solvent at 140 °C for 8 h. Preliminary investigation supported that the copper salts were also the halide sources in halogen exchange reactions. The optimized conditions are applicable to a variety of substrates and have excellent functional group tolerance. Additionally, the [BMIM]Br solvent showed good stability for at least 10 consecutive runs. Results indicated that the [BMIM]Br solvent was recyclable for reverse aromatic Finkelstein reactions.

Benefits and Limitations of Lab-on-a-Chip Method over Reversed-Phase High-Performance Liquid Chromatography Method in Gluten Proteins Evaluation

Directory of Open Access Journals (Sweden)

Dragan Živančev

2015-01-01

Full Text Available RP-HPLC (reversed-phase high-performance liquid chromatography is widely used to determine the amounts of the different gluten protein types. However, this method is time-consuming, especially at early stages of wheat breeding, when large number of samples needs to be analyzed. On the other hand, LoaC (Lab-on-a-Chip technique has the potential for a fast, reliable, and automatable analysis of proteins. In the present study, benefits and limitations of Lab-on-a-Chip method over RP-HPLC method in gluten proteins evaluation were explored in order to determine in which way LoaC method should be improved in order to make its results more compliant with the results of RP-HPLC method. Strong correlation (P≤0.001 was found between numbers of HMW glutenin peaks determined by LoaC and RP-HPLC methods. Significant correlations (P≤0.05 were obtained between percentages of HMW and LMW glutenin subunits calculated with regard to total HMW + LMW area. Even more significant correlation (P≤0.001 was found when percentages of individual HMW areas were calculated with regard to total HMW. RP-HPLC method showed superiority in determination of gliadins since larger number and better resolution of gliadin peaks were obtained by this method.

Comment on "Spontaneous liquid-liquid phase separation of water".

Science.gov (United States)

Limmer, David T; Chandler, David

2015-01-01

Yagasaki et al. [Phys. Rev. E 89, 020301 (2014)] present results from a molecular dynamics trajectory illustrating coarsening of ice, which they interpret as evidence of transient coexistence between two distinct supercooled phases of liquid water. We point out that neither two distinct liquids nor criticality are demonstrated in this simulation study. Instead, the illustrated trajectory is consistent with coarsening behaviors analyzed and predicted in earlier work by others.

A time-reversal invariant topological phase at the surface of a 3D topological insulator

International Nuclear Information System (INIS)

Bonderson, Parsa; Nayak, Chetan; Qi, Xiao-Liang

2013-01-01

A 3D fermionic topological insulator has a gapless Dirac surface state protected by time-reversal symmetry and charge conservation symmetry. The surface state can be gapped by introducing ferromagnetism to break time-reversal symmetry, introducing superconductivity to break charge conservation, or entering a topological phase. In this paper, we construct a minimal gapped topological phase that preserves both time-reversal and charge conservation symmetries and supports Ising-type non-Abelian anyons. This phase can be understood heuristically as emerging from a surface s-wave superconducting state via the condensation of eight-vortex composites. The topological phase inherits vortices supporting Majorana zero modes from the surface superconducting state. However, since it is time-reversal invariant, the surface topological phase is a distinct phase from the Ising topological phase, which can be viewed as a quantum-disordered spin-polarized p x + ip y superconductor. We discuss the anyon model of this topological phase and the manner in which time-reversal symmetry is realized in it. We also study the interfaces between the topological state and other surface gapped phases. (paper)

Non-conventional solvents in liquid phase microextraction and aqueous biphasic systems.

Science.gov (United States)

An, Jiwoo; Trujillo-Rodríguez, María J; Pino, Verónica; Anderson, Jared L

2017-06-02

The development of rapid, convenient, and high throughput sample preparation approaches such as liquid phase microextraction techniques have been continuously developed over the last decade. More recently, significant attention has been given to the replacement of conventional organic solvents used in liquid phase microextraction techniques in order to reduce toxic waste and to improve selectivity and/or extraction efficiency. With these objectives, non-conventional solvents have been explored in liquid phase microextraction and aqueous biphasic systems. The utilized non-conventional solvents include ionic liquids, magnetic ionic liquids, and deep eutectic solvents. They have been widely used as extraction solvents or additives in various liquid phase microextraction modes including dispersive liquid-liquid microextraction, single-drop microextraction, hollow fiber-liquid phase microextraction, as well as in aqueous biphasic systems. This review provides an overview into the use of non-conventional solvents in these microextraction techniques in the past 5 years (2012-2016). Analytical applications of the techniques are also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

Reversed phase chromatographic behaviour of Pu (III), Pu (IV) and Pu (VI) in presence of α-hydroxyisobutyric acid

International Nuclear Information System (INIS)

Jaison, P.G.; Telmore, V.M.; Kumar, Pranaw

2016-01-01

Understanding the aqueous chemistry of plutonium is important in process conditions as well as in environmental conditions. Since plutonium possesses multiple oxidation states which can coexist in solution, a reliable method for the identification of these oxidation states is essential to understand its physical and chemical processes. The identification of plutonium oxidation states is conventionally determined through a series of liquid-liquid extraction procedures using selective extractants. Spectroscopic and laser based techniques also have been used for the identification of its oxidation state in solutions. Liquid chromatographic behavior of different oxidation states of Pu and other actinide ions is reported to correlate their retention behaviour with stability constants. Objective of the present work is to study the reversed phase chromatography behavior of the three oxidation states of plutonium viz. Pu(III), Pu(IV) and Pu(VI) in presence of á-hydroxyisobutyric acid (HIBA) as an eluent

Development of Reverse-Phase HPLC Method for Simultaneous ...

African Journals Online (AJOL)

Erah

Purpose: To develop a simple, sensitive and rapid reverse phase HPLC method for the simultaneous analysis of metoprolol succinate and hydrochlorothiazide in a solid dosage form. Methods: The .... Extraction was carried out three times with.

Solution processing of polymer semiconductor: Insulator blends-Tailored optical properties through liquid-liquid phase separation control

KAUST Repository

Hellmann, Christoph; Treat, Neil D.; Scaccabarozzi, Alberto D.; Razzell Hollis, Joseph; Fleischli, Franziska D.; Bannock, James H.; de Mello, John; Michels, Jasper J.; Kim, Ji-Seon; Stingelin, Natalie

2014-01-01

© 2014 Wiley Periodicals, Inc. It has been demonstrated that the 0-0 absorption transition of poly(3-hexylthiophene) (P3HT) in blends with poly(ethylene oxide) (PEO) could be rationally tuned through the control of the liquid-liquid phase separation process during solution deposition. Pronounced J-like aggregation behavior, characteristic for systems of a low exciton band width, was found for blends where the most pronounced liquid-liquid phase separation occurred in solution, leading to domains of P3HT and PEO of high phase purity. Since liquid-liquid phase separation could be readily manipulated either by the solution temperature, solute concentration, or deposition temperature, to name a few parameters, our findings promise the design from the out-set of semiconductor:insulator architectures of pre-defined properties by manipulation of the interaction parameter between the solutes as well as the respective solute:solvent system using classical polymer science principles.

Solution processing of polymer semiconductor: Insulator blends-Tailored optical properties through liquid-liquid phase separation control

KAUST Repository

Hellmann, Christoph

2014-12-17

© 2014 Wiley Periodicals, Inc. It has been demonstrated that the 0-0 absorption transition of poly(3-hexylthiophene) (P3HT) in blends with poly(ethylene oxide) (PEO) could be rationally tuned through the control of the liquid-liquid phase separation process during solution deposition. Pronounced J-like aggregation behavior, characteristic for systems of a low exciton band width, was found for blends where the most pronounced liquid-liquid phase separation occurred in solution, leading to domains of P3HT and PEO of high phase purity. Since liquid-liquid phase separation could be readily manipulated either by the solution temperature, solute concentration, or deposition temperature, to name a few parameters, our findings promise the design from the out-set of semiconductor:insulator architectures of pre-defined properties by manipulation of the interaction parameter between the solutes as well as the respective solute:solvent system using classical polymer science principles.

Quality control of 99mTc-DTPA-octreotide by reverse high performance liquid chromatography

International Nuclear Information System (INIS)

Cheng, Z.; Lin, Q.F.; Jin, X.H.; Wang, F.; Bai, H.S.; Chen, D.M.; Fan, H.Q.; Du, J.

1998-01-01

DTPA-Octreotide(Pentetreotide), a somatostatin analogue which can bind specifically and with high affinity to somatostatin receptor in vitro and vivo, labeled with 99m Tc by tin reduction in acetate buffer, has been characterized by Reverse-phase High performance Liquid Chromatography. The effect of different solvents, mobile phase pH, linear gradient and the injected volume on the separation efficiency was evaluated. The results show that the separation efficiency is best using μBondapak-C 18 (300x3.9 mm 2 ), linear gradient of 40% to 80% methanol (1.0 ml/min) in 0.05M acetate buffer (pH 5.5) over a 30 min period and maintaining for another 10 min. The labeled product is a mixture which mainly consists of five components (a, b, c, d, e) successfully proved by HPLC. Paper chromatography is also evaluated in this paper. It may be used to determine the radiochemical purity of the labeling product, but is not a good choice for the verification each components. (author)

Separation of Chloroplast Pigments Using Reverse Phase Chromatography.

Science.gov (United States)

Reese, R. Neil

1997-01-01

Presents a protocol that uses reverse phase chromatography for the separation of chloroplast pigments. Provides a simple and relatively safe procedure for use in teaching laboratories. Discusses pigment extraction, chromatography, results, and advantages of the process. (JRH)

Indication of liquid-liquid phase transition in CuZr-based melts

DEFF Research Database (Denmark)

Zhou, C.; Hu, L.N.; Sun, Q.J.

2013-01-01

We study the dynamic behavior of CuZr-based melts well above the liquidus temperature. The results show a discontinuous change in viscosity during cooling, which is attributed to an underlying liquid-liquid phase transition (LLPT) in these melts. The LLPT is further verified by thermodynamic...

Vapor phase versus liquid phase grafting of meso-porous alumina

NARCIS (Netherlands)

Sripathi, V.G.P.; Mojet, Barbara; Nijmeijer, Arian; Benes, Nieck Edwin

2013-01-01

Functionalization of meso-porous c-alumina has been performed by grafting of 3-Aminopropyltrimethoxysilane (3APTMS) simultaneously from either the liquid phase or from the vapor phase. In both cases, after grafting nitrogen physisorption indicates that the materials remain meso-porous with

Fragment profiling of low molecular weight heparins using reversed phase ion pair liquid chromatography-electrospray mass spectrometry.

Science.gov (United States)

Xu, Xiaohui; Li, Daoyuan; Chi, Lequan; Du, Xuzhao; Bai, Xue; Chi, Lianli

2015-04-30

Low molecular weight heparins (LMWHs) are linear and highly charged carbohydrate polymers prepared by chemical or enzymatic depolymerization of heparin. Compared to unfractionated heparin (UFH), LMWHs are prevalently used as clinical anticoagulant drugs due to their lower side effects and better bioavailability. The work presented herein provides a rapid and powerful fragment mapping method for structural characterization of LMWHs. The chain fragments of two types of LMWHs, enoxaparin and nadroparin, were generated by controlled enzymatic digestion with each of heparinase I (Hep I, Enzyme Commission (EC) # 4.2.2.7), heparinase II (Hep II, no EC # assigned) and heparinase III (Hep III, EC # 4.2.2.8). Reversed phase ion pair high performance liquid chromatography (RPIP-HPLC) coupled with electrospray ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) was used to profile the oligosaccharide chains ranging from disaccharides to decasaccharides. A database containing all theoretical structural compositions was established to assist the mass spectra interpretation. The six digests derived by three enzymes from two types of LMWHs exhibited distinguishable fingerprinting patterns. And a total of 94 enoxaparin fragments and 109 nadroparin fragments were detected and identified. Besides the common LMWH oligosaccharides, many components containing characteristic LMWH structures such as saturated L-idopyranosuronic acid, 2,5-anhydro-D-mannitol, 1,6-anhydro-D-aminopyranose, as well as odd number oligosaccharides were also revealed. Quantitative comparison of major components derived from innovator and generic nadroparin products was presented. This approach to profile LMWHs' fragments offers a highly reproducible, high resolution and information-rich tool for evaluating the quality of this category of anticoagulant drugs or comparing structural similarities among samples from various sources. Copyright © 2015 Elsevier Ltd. All rights reserved.

Ionic liquid stationary phases for gas chromatography.

Science.gov (United States)

Poole, Colin F; Poole, Salwa K

2011-04-01

This article provides a summary of the development of ionic liquids as stationary phases for gas chromatography beginning with early work on packed columns that established details of the retention mechanism and established working methods to characterize selectivity differences compared with molecular stationary phases through the modern development of multi-centered cation and cross-linked ionic liquids for high-temperature applications in capillary gas chromatography. Since there are many reviews on ionic liquids dealing with all aspects of their chemical and physical properties, the emphasis in this article is placed on the role of gas chromatography played in the design of ionic liquids of low melting point, high thermal stability, high viscosity, and variable selectivity for separations. Ionic liquids provide unprecedented opportunities for extending the selectivity range and temperature-operating range of columns for gas chromatography, an area of separation science that has otherwise been almost stagnant for over a decade. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of related substances of telmisartan and hydrochlorothiazide in tablet dosage form by using reversed phase high performance liquid chromatographic method

Directory of Open Access Journals (Sweden)

Sutirtho Mukhopadhyay

2011-01-01

Full Text Available Objective : Telmisartan is a potent, long-lasting, nonpeptide antagonist of the angiotensin II type-1 (AT 1 receptor that is indicated for the treatment of essential hypertension. Hydrochlorothiazide is a widely prescribed diuretic and it is indicated for the treatment of edema, control of essential hypertension and management of diabetes insipidus. In the current article a new, accurate, sensitive, precise, rapid, reversed phase high performance liquid chromatography (RP-HPLC method was developed for determination of related substances of Telmisartan and Hydrochlorthiazide in tablet dosage form. Materials and Methods : Simultaneous determination of related substances was performed on Kromasil C 18 analytical column (250 × 4.6 mm; 5΅m pertical size column at 40°C employing a gradient elution. Mobile phase consisting of solvent A (solution containing 2.0 g of potassium dihydrogen phosphate anhydrous and 1.04 g of Sodium 1- Hexane sulphonic acid monohydrate per liter of water, adjusted to pH 3.0 with orthophosphoric acid and solvent B (mixture of Acetonitrile: Methanol in the ratio 80:20 v/v was used at a flow rate of 1.0 ml min−1 . UV detection was performed at 270 nm. Results : During method validation parameter such as precision, linearity, accuracy, specificity, limit of detection and quantification were evaluated, which remained within acceptable limits. Conclusions : HPLC analytical method is linear, accurate, precise, robust and specific, being able to separate the main drug from its degradation products. It may find application for the routine analysis of the related substances of both Telmisartan and Hydrochlorthiazide in this combination tablets.

Comment on "Spontaneous liquid-liquid phase separation of water"

Science.gov (United States)

Limmer, David T.; Chandler, David

2015-01-01

Yagasaki et al. [Phys. Rev. E 89, 020301 (2014), 10.1103/PhysRevE.89.020301] present results from a molecular dynamics trajectory illustrating coarsening of ice, which they interpret as evidence of transient coexistence between two distinct supercooled phases of liquid water. We point out that neither two distinct liquids nor criticality are demonstrated in this simulation study. Instead, the illustrated trajectory is consistent with coarsening behaviors analyzed and predicted in earlier work by others.

Nanomaterials as stationary phases and supports in liquid chromatography.

Science.gov (United States)

Beeram, Sandya R; Rodriguez, Elliott; Doddavenkatanna, Suresh; Li, Zhao; Pekarek, Allegra; Peev, Darin; Goerl, Kathryn; Trovato, Gianfranco; Hofmann, Tino; Hage, David S

2017-10-01

The development of various nanomaterials over the last few decades has led to many applications for these materials in liquid chromatography (LC). This review will look at the types of nanomaterials that have been incorporated into LC systems and the applications that have been explored for such systems. A number of carbon-based nanomaterials and inorganic nanomaterials have been considered for use in LC, ranging from carbon nanotubes, fullerenes and nanodiamonds to metal nanoparticles and nanostructures based on silica, alumina, zirconia and titanium dioxide. Many ways have been described for incorporating these nanomaterials into LC systems. These methods have included covalent immobilization, adsorption, entrapment, and the synthesis or direct development of nanomaterials as part of a chromatographic support. Nanomaterials have been used in many types of LC. These applications have included the reversed-phase, normal-phase, ion-exchange, and affinity modes of LC, as well as related methods such as chiral separations, ion-pair chromatography and hydrophilic interaction liquid chromatography. Both small and large analytes (e.g., dyes, drugs, amino acids, peptides and proteins) have been used to evaluate possible applications for these nanomaterial-based methods. The use of nanomaterials in columns, capillaries and planar chromatography has been considered as part of these efforts. Potential advantages of nanomaterials in these applications have included their good chemical and physical stabilities, the variety of interactions many nanomaterials can have with analytes, and their unique retention properties in some separation formats. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

FORTRAN program for calculating liquid-phase and gas-phase thermal diffusion column coefficients

International Nuclear Information System (INIS)

Rutherford, W.M.

1980-01-01

A computer program (COLCO) was developed for calculating thermal diffusion column coefficients from theory. The program, which is written in FORTRAN IV, can be used for both liquid-phase and gas-phase thermal diffusion columns. Column coefficients for the gas phase can be based on gas properties calculated from kinetic theory using tables of omega integrals or on tables of compiled physical properties as functions of temperature. Column coefficients for the liquid phase can be based on compiled physical property tables. Program listings, test data, sample output, and users manual are supplied for appendices

A reversed-phase compatible thin-layer chromatography autography for the detection of acetylcholinesterase inhibitors.

Science.gov (United States)

Ramallo, I Ayelen; García, Paula; Furlan, Ricardo L E

2015-11-01

A dual readout autographic assay to detect acetylcholinesterase inhibitors present in complex matrices adsorbed on reversed-phase or normal-phase thin-layer chromatography plates is described. Enzyme gel entrapment with an amphiphilic copolymer was used for assay development. The effects of substrate and enzyme concentrations, pH, incubation time, and incubation temperature on the sensitivity and the detection limit of the assay were evaluated. Experimental design and response surface methodology were used to optimize conditions with a minimum number of experiments. The assay allowed the detection of 0.01% w/w of physostigmine in both a spiked Sonchus oleraceus L. extract chromatographed on normal phase and a spiked Pimenta racemosa (Mill.) J.W. Moore leaf essential oil chromatographed on reversed phase. Finally, the reversed-phase thin-layer chromatography assay was applied to reveal the presence of an inhibitor in the Cymbopogon citratus (DC.) Stapf essential oil. The developed assay is able to detect acetylcholinesterase inhibitors present in complex matrixes that were chromatographed in normal phase or reversed-phase thin-layer chromatography. The detection limit for physostigmine on both normal and reversed phase was of 1×10(-4) μg. The results can be read by a change in color and/or a change in fluorescence. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Continuous fixed-bed gas-phase hydroformylation using supported ionic liquid-phase (SILP) Rh catalysts

DEFF Research Database (Denmark)

Riisager, Anders; Wasserscheid, Peter; Van Hal, R.

2003-01-01

Continuous flow gas-phase hydroformylation of propene was performed using novel supported ionic liquid-phase (SILP) catalysts containing immobilized Rh complexes of the biphosphine ligand sulfoxantphos in the ionic liquids 1-n-butyl-3-methylimidazolium hexafluorophosphate and halogen-free 1-n-butyl...

Structure analysis of turbulent liquid phase by POD and LSE techniques

International Nuclear Information System (INIS)

Munir, S.; Muthuvalu, M. S.; Siddiqui, M. I.; Heikal, M. R.; Aziz, A. Rashid A.

2014-01-01

In this paper, vortical structures and turbulence characteristics of liquid phase in both single liquid phase and two-phase slug flow in pipes were studied. Two dimensional velocity vector fields of liquid phase were obtained by Particle image velocimetry (PIV). Two cases were considered one single phase liquid flow at 80 l/m and second slug flow by introducing gas at 60 l/m while keeping liquid flow rate same. Proper orthogonal decomposition (POD) and Linear stochastic estimation techniques were used for the extraction of coherent structures and analysis of turbulence in liquid phase for both cases. POD has successfully revealed large energy containing structures. The time dependent POD spatial mode coefficients oscillate with high frequency for high mode numbers. The energy distribution of spatial modes was also achieved. LSE has pointed out the coherent structured for both cases and the reconstructed velocity fields are in well agreement with the instantaneous velocity fields

Structure analysis of turbulent liquid phase by POD and LSE techniques

Energy Technology Data Exchange (ETDEWEB)

Munir, S., E-mail: shahzad-munir@comsats.edu.pk; Muthuvalu, M. S.; Siddiqui, M. I. [Department of Fundamental and Applied Science, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750 Tronoh, Perak Darul Ridzuan (Malaysia); Heikal, M. R., E-mail: morgan.heikal@petronas.com.my; Aziz, A. Rashid A., E-mail: morgan.heikal@petronas.com.my [Department of Mechanical Engineering, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750 Tronoh, Perak Darul Ridzuan (Malaysia)

2014-10-24

In this paper, vortical structures and turbulence characteristics of liquid phase in both single liquid phase and two-phase slug flow in pipes were studied. Two dimensional velocity vector fields of liquid phase were obtained by Particle image velocimetry (PIV). Two cases were considered one single phase liquid flow at 80 l/m and second slug flow by introducing gas at 60 l/m while keeping liquid flow rate same. Proper orthogonal decomposition (POD) and Linear stochastic estimation techniques were used for the extraction of coherent structures and analysis of turbulence in liquid phase for both cases. POD has successfully revealed large energy containing structures. The time dependent POD spatial mode coefficients oscillate with high frequency for high mode numbers. The energy distribution of spatial modes was also achieved. LSE has pointed out the coherent structured for both cases and the reconstructed velocity fields are in well agreement with the instantaneous velocity fields.

High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids

DEFF Research Database (Denmark)

Lue, Bena-Marie; Guo, Zheng; Xu, X.B.

2008-01-01

Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found...... essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method...

Modelling of retention of pesticides in reversed-phase high-performance liquid chromatography: Quantitative structure-retention relationships based on solute quantum-chemical descriptors and experimental (solvatochromic and spin-probe) mobile phase descriptors

International Nuclear Information System (INIS)

D'Archivio, Angelo Antonio; Ruggieri, Fabrizio; Mazzeo, Pietro; Tettamanti, Enzo

2007-01-01

A quantitative structure-retention relationship (QSRR) analysis based on multilinear regression (MLR) and artificial neural networks (ANNs) is carried out to model the combined effect of solute structure and eluent composition on the retention behaviour of pesticides in isocratic reversed-phase high-performance liquid chromatography (RP-HPLC). The octanol-water partition coefficient and four quantum chemical descriptors (the total dipole moment, the mean polarizability, the anisotropy of the polarizability and a descriptor of hydrogen-bonding based on the atomic charges on acidic and basic chemical functionalities) are considered as solute descriptors. In order to identify suitable mobile phase descriptors, encoding composition-dependent properties of both methanol- and acetonitrile-containing mobile phases, the Kamlet-Taft solvatochromic parameters (polarity-dipolarity, hydrogen-bond acidity and hydrogen-bond basicity, π * , α and β, respectively) and the 14 N hyperfine-splitting constant (a N ) of a spin-probe dissolved in the eluent are examined. A satisfactory description of mobile phase properties influencing the solute retention is provided by a N and β or alternatively π * and β. The two seven-parameter models resulting from combination of a N and β, or π * and β, with the solute descriptors were tested on a set of 26 pesticides representative of 10 different chemical classes in a wide range of mobile phase composition (30-60% (v/v) water-methanol and 30-70% (v/v) water-acetonitrile). Within the explored experimental range, the acidity of the eluent, as quantified by α, is almost constant, and this parameter is in fact irrelevant. The results reveal that a N and π * , that can be considered as interchangeable mobile phase descriptors, are the most influent variables in the respective models. The predictive ability of the proposed models, as tested on an external data set, is quite good (Q 2 close to 0.94) when a MLR approach is used, but the

Modelling of retention of pesticides in reversed-phase high-performance liquid chromatography: Quantitative structure-retention relationships based on solute quantum-chemical descriptors and experimental (solvatochromic and spin-probe) mobile phase descriptors

Energy Technology Data Exchange (ETDEWEB)

D' Archivio, Angelo Antonio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy)]. E-mail: darchivi@univaq.it; Ruggieri, Fabrizio [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); Mazzeo, Pietro [Dipartimento di Chimica, Ingegneria Chimica e Materiali, Universita degli Studi di L' Aquila, Via Vetoio, 67010 Coppito, L' Aquila (Italy); Tettamanti, Enzo [Dipartimento di Scienze Biomediche Comparate, Universita di Teramo, P.zzale A. Moro 45, 64100 Teramo (Italy)

2007-06-19

A quantitative structure-retention relationship (QSRR) analysis based on multilinear regression (MLR) and artificial neural networks (ANNs) is carried out to model the combined effect of solute structure and eluent composition on the retention behaviour of pesticides in isocratic reversed-phase high-performance liquid chromatography (RP-HPLC). The octanol-water partition coefficient and four quantum chemical descriptors (the total dipole moment, the mean polarizability, the anisotropy of the polarizability and a descriptor of hydrogen-bonding based on the atomic charges on acidic and basic chemical functionalities) are considered as solute descriptors. In order to identify suitable mobile phase descriptors, encoding composition-dependent properties of both methanol- and acetonitrile-containing mobile phases, the Kamlet-Taft solvatochromic parameters (polarity-dipolarity, hydrogen-bond acidity and hydrogen-bond basicity, {pi} {sup *}, {alpha} and {beta}, respectively) and the {sup 14}N hyperfine-splitting constant (a {sub N}) of a spin-probe dissolved in the eluent are examined. A satisfactory description of mobile phase properties influencing the solute retention is provided by a {sub N} and {beta} or alternatively {pi} {sup *} and {beta}. The two seven-parameter models resulting from combination of a {sub N} and {beta}, or {pi} {sup *} and {beta}, with the solute descriptors were tested on a set of 26 pesticides representative of 10 different chemical classes in a wide range of mobile phase composition (30-60% (v/v) water-methanol and 30-70% (v/v) water-acetonitrile). Within the explored experimental range, the acidity of the eluent, as quantified by {alpha}, is almost constant, and this parameter is in fact irrelevant. The results reveal that a {sub N} and {pi} {sup *}, that can be considered as interchangeable mobile phase descriptors, are the most influent variables in the respective models. The predictive ability of the proposed models, as tested on an

Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

Energy Technology Data Exchange (ETDEWEB)

MarszaII, MichaI Piotr [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Baczek, Tomasz [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Kaliszan, Roman [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland)]. E-mail: roman.kaliszan@amg.gda.pl

2005-08-22

A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development.

Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

International Nuclear Information System (INIS)

MarszaII, MichaI Piotr; Baczek, Tomasz; Kaliszan, Roman

2005-01-01

A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development

Diazonium modification of porous graphitic carbon with catechol and amide groups for hydrophilic interaction and attenuated reversed phase liquid chromatography.

Science.gov (United States)

Iverson, Chad D; Zhang, Ya; Lucy, Charles A

2015-11-27

Porous graphitic carbon (PGC) is an increasingly popular and attractive phase for HPLC on account of its chemical and thermal stability, and its unique separation mechanism. However, native PGC is strongly hydrophobic and in some instances excessively retentive. As part of our effort to build a library of hydrophilic covalently modified PGC phases, we functionalized PGC with catechol and amide groups by means of aryl diazonium chemistry to produce two new phases. Successful grafting was confirmed by X-ray photoelectron spectroscopy (XPS). Under HILIC conditions, the Catechol-PGC showed up to 5-fold increased retention relative to unmodified PGC and selectivity that differed from four other HILIC phases. Under reversed phase conditions, the Amide-PGC reduced the retentivity of PGC by almost 90%. The chromatographic performance of Catechol-PGC and Amide-PGC is demonstrated by separations of nucleobases, nucleosides, phenols, alkaline pharmaceuticals, and performance enhancing stimulants. These compounds had retention factors (k) ranging from 0.5 to 13. Copyright © 2015 Elsevier B.V. All rights reserved.

C18, C8, and perfluoro reversed phases on diamond for solid-phase extraction.

Science.gov (United States)

Saini, Gaurav; Wiest, Landon A; Herbert, David; Biggs, Katherine N; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

2009-04-17

In spite of advances in solid-phase extraction (SPE) technology there are certain disadvantages to current SPE silica-based, column packings. The pH range over which extraction can occur is limited and each column is generally only used once. New diamond-based reversed SPE phases (C(18), C(8), and perfluorinated) were developed in our laboratories. Studies were done which show that these phases do not have the same limitations as traditional silica-based stationary phases. The synthesis and properties of these diamond-based phases are presented, and the stability, percent recovery, and column capacity are given for the C(18) phase.

Analysis of phosphorus herbicides by ion-pairing reversed-phase liquid chromatography coupled to inductively coupled plasma mass spectrometry with octapole reaction cell.

Science.gov (United States)

Sadi, Baki B M; Vonderheide, Anne P; Caruso, Joseph A

2004-09-24

A reversed phase ion-pairing high performance liquid chromatographic (RPIP-HPLC) method is developed for the separation of two phosphorus herbicides, Glufosinate and Glyphosate as well as Aminomethylphosphonic acid (AMPA), the major metabolite of Glyphosate. Tetrabutylammonium hydroxide is used as the ion-pairing reagent in conjunction with an ammonium acetate/acetic acid buffering system at pH 4.7. An inductively coupled plasma mass spectrometer (ICP-MS) is coupled to the chromatographic system to detect the herbicides at m/z = 31P. Historically, phosphorus has been recognized as one of the elements difficult to analyze in argon plasma. This is due to its relatively high ionization potential (10.5 eV) as well as the inherent presence of the polyatomic interferences 14N16O1H+ and 15N16O+ overlapping its only isotope at m/z = 31. An octapole reaction cell is utilized to minimize the isobaric polyatomic interferences and to obtain the highest signal-to-background ratio. Detection limits were found to be in the low ppt range (25-32 ng/l). The developed method is successfully applied to the analysis of water samples collected from the Ohio River and spiked with a standard compounds at a level of 20 microg/l.

The nuclear liquid gas phase transition and phase coexistence

International Nuclear Information System (INIS)

Chomaz, Ph.

2001-01-01

In this talk we will review the different signals of liquid gas phase transition in nuclei. From the theoretical side we will first discuss the foundations of the concept of equilibrium, phase transition and critical behaviors in infinite and finite systems. From the experimental point of view we will first recall the evidences for some strong modification of the behavior of hot nuclei. Then we will review quantitative detailed analysis aiming to evidence phase transition, to define its order and phase diagram. Finally, we will present a critical discussion of the present status of phase transitions in nuclei and we will draw some lines for future development of this field. (author)

The nuclear liquid gas phase transition and phase coexistence

Energy Technology Data Exchange (ETDEWEB)

Chomaz, Ph

2001-07-01

In this talk we will review the different signals of liquid gas phase transition in nuclei. From the theoretical side we will first discuss the foundations of the concept of equilibrium, phase transition and critical behaviors in infinite and finite systems. From the experimental point of view we will first recall the evidences for some strong modification of the behavior of hot nuclei. Then we will review quantitative detailed analysis aiming to evidence phase transition, to define its order and phase diagram. Finally, we will present a critical discussion of the present status of phase transitions in nuclei and we will draw some lines for future development of this field. (author)

Manipulating Liquids With Acoustic Radiation Pressure Phased Arrays

Science.gov (United States)

Oeftering, Richard C.

1999-01-01

High-intensity ultrasound waves can produce the effects of "Acoustic Radiation Pressure" (ARP) and "acoustic streaming." These effects can be used to propel liquid flows and to apply forces that can be used to move or manipulate floating objects or liquid surfaces. NASA's interest in ARP includes the remote-control agitation of liquids and the manipulation of bubbles and drops in liquid experiments and propellant systems. A high level of flexibility is attained by using a high-power acoustic phased array to generate, steer, and focus a beam of acoustic waves. This is called an Acoustic Radiation Pressure Phased Array, or ARPPA. In this approach, many acoustic transducer elements emit wavelets that converge into a single beam of sound waves. Electronically coordinating the timing, or "phase shift," of the acoustic waves makes it possible to form a beam with a predefined direction and focus. Therefore, a user can direct the ARP force at almost any desired point within a liquid volume. ARPPA lets experimenters manipulate objects anywhere in a test volume. This flexibility allow it to be used for multiple purposes, such as to agitate liquids, deploy and manipulate drops or bubbles, and even suppress sloshing in spacecraft propellant tanks.

Analysis of nine food additives in red wine by ion-suppression reversed-phase high-performance liquid chromatography using trifluoroacetic acid and ammonium acetate as ion-suppressors.

Science.gov (United States)

Zhao, Yong-Gang; Chen, Xiao-Hong; Yao, Shan-Shan; Pan, Sheng-Dong; Li, Xiao-Ping; Jin, Mi-Cong

2012-01-01

A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in red wine. The effects of ion-suppressors, i.e., trifluoroacetic acid (TFA) and ammonium acetate (AmAc) on retention behavior of nine food additives in RP-HPLC separation were discussed in detail. The relationships between retention factors of solutes and volume percent of ion-suppressors in the mobile-phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, respectively. The results showed that the ion suppressors had not only an ion suppression effect, but also an organic modification effect on the acidic analytes. The baseline separation of nine food additives was completed by a gradient elution with acetonitrile-TFA(0.01%, v/v)-AmAc(2.5 mmol L(-1)) aqueous solution as the mobile phase. The recoveries were between 80.2 - 99.5% for all analytes with RSDs in the range of 1.5 - 8.9%. The linearities were in the range of 0.2 - 100.0 mg L(-1) with determination coefficients (r(2)) higher than 0.9991 for all analytes. The limits of quantification (LOQs) were between 0.53 - 0.99 mg L(-1). The applicability of the proposed method to detect and quantify food additives has been demonstrated in the analysis of 30 real samples.

Radiation degradation of waste waters. Reverse phase-high performance liquid chromatography and multicomponent UV-VIS analysis of gamma-irradiated aqueous solutions of nitrobenzene Pt.1

International Nuclear Information System (INIS)

Kuruc, J.; Sahoo, M.K.; Locaj, J.; Hutta, M.

1994-01-01

Saturated aqueous solutions of nitrobenzene (in water, 0.1M nitric acid and 0.1M potassium hydroxide) were irradiated with 60 Co γ-rays in deaerated condition. Radiolytic products were analyzed using reverse phase-high performance liquid chromatography (RP-HPLC) and multicomponent UV-VIS spectrometry. With the aid of RP-HPLC retention times of the radiolytic products were found to be identical with those of isomeric nitrophenols, aminophenols and dinitrophenols. According to the primary information obtained from RP-HPLC and literature, we have chosen ten standards and eleven wavelengths for multicomponent UV-VIS analysis (linear multiparametric regression analysis) and the concentrations of nitrobenzene, nitrophenols, aminophenols and dinitrophenols in water, HNO 3 and KOH solutions were calculated. G-values (molecules/100 eV) of the radiolytic products and decomposition of nitrobenzene in aqueous solutions G(-nitrobenzene) were calculated from the dependence of their concentrations with dose. Ph has relatively little influence on the decrease of concentration of nitrobenzene, but has strong influence on the product composition. (author) 7 refs.; 5 figs.; 5 tabs

Visualization and measurement of liquid velocity field of gas-liquid metal two-phase flow using neutron radiography

International Nuclear Information System (INIS)

Saito, Yasushi; Suzuki, Tohru; Matsubayashi, Masahito

2000-01-01

In a core melt accident of a fast breeder reactor, a possibility of re-criticality is anticipated in the molten fuel-steel mixture pool. One of the mechanisms to suppress the re-criticality is the boiling of steel in the molten fuel-steel mixture pool because of the negative void reactivity effect. To evaluate the reactivity change due to boiling, it is necessary to know the characteristics of gas-liquid two-phase flow in the molten fuel-steel mixture pool. For this purpose, boiling bubbles in a molten fuel-steel mixture pool were simulated by adiabatic gas bubbles in a liquid metal pool to study the basic characteristics of gas-liquid metal two-phase mixture. Visualization of the two-phase mixture and measurements of liquid phase velocity and void fraction were conducted by using neutron radiography and image processing techniques. From these measurements, the basic characteristics of gas-liquid metal two-phase mixture were clarified. (author)

How ionic species structure influences phase structure and transitions from protic ionic liquids to liquid crystals to crystals.

Science.gov (United States)

Greaves, Tamar L; Broomhall, Hayden; Weerawardena, Asoka; Osborne, Dale A; Canonge, Bastien A; Drummond, Calum J

2017-12-14

The phase behaviour of n-alkylammonium (C6 to C16) nitrates and formates has been characterised using synchrotron small angle and wide angle X-ray scattering (SAXS/WAXS), differential scanning calorimetry (DSC), cross polarised optical microscopy (CPOM) and Fourier transform infrared spectroscopy (FTIR). The protic salts may exist as crystalline, liquid crystalline or ionic liquid materials depending on the alkyl chain length and temperature. n-Alkylammonium nitrates with n ≥ 6 form thermotropic liquid crystalline (LC) lamellar phases, whereas n ≥ 8 was required for the formate series to form this LC phase. The protic ionic liquid phase showed an intermediate length scale nanostructure resulting from the segregation of the polar and nonpolar components of the ionic liquid. This segregation was enhanced for longer n-alkyl chains, with a corresponding increase in the correlation length scale. The crystalline and liquid crystalline phases were both lamellar. Phase transition temperatures, lamellar d-spacings, and liquid correlation lengths for the n-alkylammonium nitrates and formates were compared with those for n-alkylammonium chlorides and n-alkylamines. Plateau regions in the liquid crystalline to liquid phase transition temperatures as a function of n for the n-alkylammonium nitrates and formates are consistent with hydrogen-bonding and cation-anion interactions between the ionic species dominating alkyl chain-chain van der Waals interactions, with the exception of the mid chained hexyl- and heptylammonium formates. The d-spacings of the lamellar phases for both the n-alkylammonium nitrates and formates were consistent with an increase in chain-chain layer interdigitation within the bilayer-based lamellae with increasing alkyl chain length, and they were comparable to the n-alkylammonium chlorides.

Synthetically chemical-electrical mechanism for controlling large scale reversible deformation of liquid metal objects

Science.gov (United States)

Zhang, Jie; Sheng, Lei; Liu, Jing

2014-11-01

Reversible deformation of a machine holds enormous promise across many scientific areas ranging from mechanical engineering to applied physics. So far, such capabilities are still hard to achieve through conventional rigid materials or depending mainly on elastomeric materials, which however own rather limited performances and require complicated manipulations. Here, we show a basic strategy which is fundamentally different from the existing ones to realize large scale reversible deformation through controlling the working materials via the synthetically chemical-electrical mechanism (SCHEME). Such activity incorporates an object of liquid metal gallium whose surface area could spread up to five times of its original size and vice versa under low energy consumption. Particularly, the alterable surface tension based on combination of chemical dissolution and electrochemical oxidation is ascribed to the reversible shape transformation, which works much more flexible than many former deformation principles through converting electrical energy into mechanical movement. A series of very unusual phenomena regarding the reversible configurational shifts are disclosed with dominant factors clarified. This study opens a generalized way to combine the liquid metal serving as shape-variable element with the SCHEME to compose functional soft machines, which implies huge potential for developing future smart robots to fulfill various complicated tasks.

Optical reversible programmable Boolean logic unit.

Science.gov (United States)

Chattopadhyay, Tanay

2012-07-20

Computing with reversibility is the only way to avoid dissipation of energy associated with bit erase. So, a reversible microprocessor is required for future computing. In this paper, a design of a simple all-optical reversible programmable processor is proposed using a polarizing beam splitter, liquid crystal-phase spatial light modulators, a half-wave plate, and plane mirrors. This circuit can perform 16 logical operations according to three programming inputs. Also, inputs can be easily recovered from the outputs. It is named the "reversible programmable Boolean logic unit (RPBLU)." The logic unit is the basic building block of many complex computational operations. Hence the design is important in sense. Two orthogonally polarized lights are defined here as two logical states, respectively.

Tube Radial Distribution Flow Separation in a Microchannel Using an Ionic Liquid Aqueous Two-Phase System Based on Phase Separation Multi-Phase Flow.

Science.gov (United States)

Nagatani, Kosuke; Shihata, Yoshinori; Matsushita, Takahiro; Tsukagoshi, Kazuhiko

2016-01-01

Ionic liquid aqueous two-phase systems were delivered into a capillary tube to achieve tube radial distribution flow (TRDF) or annular flow in a microspace. The phase diagram, viscosity of the phases, and TRDF image of the 1-butyl-3-methylimidazolium chloride and NaOH system were examined. The TRDF was formed with inner ionic liquid-rich and outer ionic liquid-poor phases in the capillary tube. The phase configuration was explained using the viscous dissipation principle. We also examined the distribution of rhodamine B in a three-branched microchannel on a microchip with ionic liquid aqueous two-phase systems for the first time.

The use of Fourier reverse transforms in crystallographic phase refinement

Energy Technology Data Exchange (ETDEWEB)

Ringrose, Sharon [Iowa State Univ., Ames, IA (United States)

1997-10-08

Often a crystallographer obtains an electron density map which shows only part of the structure. In such cases, the phasing of the trial model is poor enough that the electron density map may show peaks in some of the atomic positions, but other atomic positions are not visible. There may also be extraneous peaks present which are not due to atomic positions. A method for determination of crystal structures that have resisted solution through normal crystallographic methods has been developed. PHASER is a series of FORTRAN programs which aids in the structure solution of poorly phased electron density maps by refining the crystallographic phases. It facilitates the refinement of such poorly phased electron density maps for difficult structures which might otherwise not be solvable. The trial model, which serves as the starting point for the phase refinement, may be acquired by several routes such as direct methods or Patterson methods. Modifications are made to the reverse transform process based on several assumptions. First, the starting electron density map is modified based on the fact that physically the electron density map must be non-negative at all points. In practice a small positive cutoff is used. A reverse Fourier transform is computed based on the modified electron density map. Secondly, the authors assume that a better electron density map will result by using the observed magnitudes of the structure factors combined with the phases calculated in the reverse transform. After convergence has been reached, more atomic positions and less extraneous peaks are observed in the refined electron density map. The starting model need not be very large to achieve success with PHASER; successful phase refinement has been achieved with a starting model that consists of only 5% of the total scattering power of the full molecule. The second part of the thesis discusses three crystal structure determinations.

[Determination of ciprofloxacin in human serum and urine by reversed-phase HPLC].

Science.gov (United States)

Qin, Y; Liang, D

1993-03-01

A sensitive and rapid method for the determination of ciprofloxacin using enoxacin as the internal standard was reported. High-performance liquid chromatograph model 344 (Beckman, USA) with a variable wavelength UV detector and reversed-phase Ultrasphere-ODS column (5 microns, 250 x 4.6 mm) was used. Serum or urine sample preparation involved addition phosphate buffer (pH 7.5) and aqueous solution of sodium lauryl sulfate, followed by chloroform extraction. The organic layer was removed and evaporated to dryness under an air stream in a 37 degrees C water bath. The residue was dissolved in 50 microliters mobile phase and 20 microliters injected. The mobile phase of 0.02 mol/L acetate buffer (pH 3.0) -acetonitril-dimethylformamide-10% aqueous solution of tetrabutyl ammonium hydroxide (88:6.5:5:0.5) was pumped at 0.9 ml/min through the column. The detector operated at 0.01 aufs and the wavelength was set at 276 nm. The retention times for ciprofloxacin and enoxacin were 7.31 min and 5.59 min, respectively. In serum, standard curve was linear in the concentration range of 0.75 to 24 mumol/L, the detective limit was 0.2 mumol/L, extraction recovery was 69-74%, within-day CV was less than 5%, and inter-day CV was less than 6%.

CO2 Capture with Liquid-Liquid Phase Change Solvents: A Thermodynamic Study

DEFF Research Database (Denmark)

Waseem Arshad, Muhammad; Fosbøl, Philip Loldrup; von Solms, Nicolas

2017-01-01

by the quaternary H2O-DEEAMAPA-CO2 system which gives liquid-liquid phase split when reacted with carbon dioxide. A total of 94 model parameters and 6 thermodynamic properties were fitted to approximately 1500 equilibrium and thermal experimental data consisting of pureamine vapor pressure (Pvap), vapor...

Liquid phase chromatography on microchips

DEFF Research Database (Denmark)

Kutter, Jörg Peter

2012-01-01

explosive development of, in particular, chromatographic separation systems on microchips, has, however, slowed down in recent years. This review takes a closer, critical look at how liquid phase chromatography has been implemented in miniaturized formats over the past several years, what is important...

Simultaneous determination of F-beta-alanine and beta-alanine in plasma and urine with dual-column reversed-phase high-performance liquid chromatography

NARCIS (Netherlands)

van Kuilenburg, A. B.; Stroomer, A. E.; Peters, G. J.; van Gennip, A. H.

2001-01-01

F-beta-Alanine and beta-alanine were detected in plasma and urine samples with fluorescence detection of orthophthaldialdehyde derivatives of F-beta-alanine and beta-alanine after separation with dual-column reversed-phase HPLC. The detection limits of F-beta-alanine and beta-alanine in the HPLC

Phase retrieval with the reverse projection method in the presence of object's scattering

International Nuclear Information System (INIS)

Wang, Zhili; Gao, Kun; Wang, Dajiang

2017-01-01

X-ray grating interferometry can provide substantially increased contrast over traditional attenuation-based techniques in biomedical applications, and therefore novel and complementary information. Recently, special attention has been paid to quantitative phase retrieval in X-ray grating interferometry, which is mandatory to perform phase tomography, to achieve material identification, etc. An innovative approach, dubbed “Reverse Projection” (RP), has been developed for quantitative phase retrieval. The RP method abandons grating scanning completely, and is thus advantageous in terms of higher efficiency and reduced radiation damage. Therefore, it is expected that this novel method would find its potential in preclinical and clinical implementations. Strictly speaking, the reverse projection method is applicable for objects exhibiting only absorption and refraction. In this contribution, we discuss the phase retrieval with the reverse projection method for general objects with absorption, refraction and scattering simultaneously. Especially, we investigate the influence of the object's scattering on the retrieved refraction signal. Both theoretical analysis and numerical experiments are performed. The results show that the retrieved refraction signal is the product of object's refraction and scattering signals for small values. In the case of a strong scattering, the reverse projection method cannot provide reliable phase retrieval. Those presented results will guide the use of the reverse projection method for future practical applications, and help to explain some possible artifacts in the retrieved images and/or reconstructed slices. - Highlights: • Accurate phase retrieval by the reverse projection method without object's scattering. • Retrieved refraction signal contaminated by the object's scattering. • Refraction signal underestimated by the reverse projection method. • Guide the use of the reverse projection method for

Application of reverse osmosis to the treatment of liquid effluents produced by nuclear power plants

International Nuclear Information System (INIS)

Huet, Y.; Poulat, B.; Menjeaud, C.

1989-01-01

Radioactive liquid effluents generated during the operation of PWR nuclear power units are currently treated by two independent systems. The effluents from the reactor coolant system are recycled, unlike the others, which, after treatment, are released into the river or ocean that provides cooling water for the unit. The objective of the treatment of nonrecycled effluents is to separate from them as much of the radioactive particles that they contain as possible, so as to release into the environment a maximum volume of nonradioactive waste, and to be left with only a minimum volume of concentrated waste, containing most of the initial radioactivity, which must be loaded into casks for storage. Membrane-based filtration techniques, because they have excellent separation performances, can logically be used for this decontamination of the liquid effluents. Having developed its own reverse osmosis membrane, a possible application in a nuclear power plant, i.e., integration of a reverse osmosis unit into a radioactive liquid effluent treatment system is presented. (author)

Balance of liquid-phase turbulence kinetic energy equation for bubble-train flow

International Nuclear Information System (INIS)

Ilic, Milica; Woerner, Martin; Cacuci, Dan Gabriel

2004-01-01

In this paper the investigation of bubble-induced turbulence using direct numerical simulation (DNS) of bubbly two-phase flow is reported. DNS computations are performed for a bubble-driven liquid motion induced by a regular train of ellipsoidal bubbles rising through an initially stagnant liquid within a plane vertical channel. DNS data are used to evaluate balance terms in the balance equation for the liquid phase turbulence kinetic energy. The evaluation comprises single-phase-like terms (diffusion, dissipation and production) as well as the interfacial term. Special emphasis is placed on the procedure for evaluation of interfacial quantities. Quantitative analysis of the balance equation for the liquid phase turbulence kinetic energy shows the importance of the interfacial term which is the only source term. The DNS results are further used to validate closure assumptions employed in modelling of the liquid phase turbulence kinetic energy transport in gas-liquid bubbly flows. In this context, the performance of respective closure relations in the transport equation for liquid turbulence kinetic energy within the two-phase k-ε and the two-phase k-l model is evaluated. (author)

Highly Selective Continuous Gas-Phase Methoxycarbonylation of Ethylene with Supported Ionic Liquid Phase (SILP) Catalysts

DEFF Research Database (Denmark)

Khokarale, Santosh Govind; Garcia Suárez, Eduardo José; Fehrmann, Rasmus

2017-01-01

Supported ionic liquid phase (SILP) technology was applied for the first time to the Pd-catalyzed continuous, gas-phase methoxycarbonylation of ethylene to selectively produce methyl propanoate (MP) in high yields. The influence of catalyst and reaction parameters such as, for example, ionic liquid...

Comparison of cryopreserved human sperm in vapor and liquid phases of liquid nitrogen: effect on motility parameters, morphology, and sperm function.

Science.gov (United States)

Punyatanasakchai, Piyaphan; Sophonsritsuk, Areephan; Weerakiet, Sawaek; Wansumrit, Surapee; Chompurat, Deonthip

2008-11-01

To compare the effects of cryopreserved sperm in vapor and liquid phases of liquid nitrogen on sperm motility, morphology, and sperm function. Experimental study. Andrology laboratory at Ramathibodi Hospital, Thailand. Thirty-eight semen samples with normal motility and sperm count were collected from 38 men who were either patients of an infertility clinic or had donated sperm for research. Each semen sample was divided into two aliquots. Samples were frozen with static-phase vapor cooling. One aliquot was plunged into liquid nitrogen (-196 degrees C), and the other was stored in vapor-phase nitrogen (-179 degrees C) for 3 days. Thawing was performed at room temperature. Motility was determined by using computer-assisted semen analysis, sperm morphology was determined by using eosin-methylene blue staining, and sperm function was determined by using a hemizona binding test. Most of the motility parameters of sperm stored in the vapor phase were not significantly different from those stored in the liquid phase of liquid nitrogen, except in amplitude of lateral head displacement. The percentages of normal sperm morphology in both vapor and liquid phases also were not significantly different. There was no significant difference in the number of bound sperm in hemizona between sperm cryopreserved in both vapor and liquid phases of liquid nitrogen. Cryopreservation of human sperm in a vapor phase of liquid nitrogen was comparable to cryopreservation in a liquid phase of liquid nitrogen.

Determination of phenyl-N-methylcarbamates and their hydrolysis products in water, using solid-phase extraction and reversed-phase liquid chromatography with UV and electrospray mass spectrometric detection

International Nuclear Information System (INIS)

El Atrache, L.L.; Sabbah, S.

2003-01-01

In this study, eight phenyl-N-methylcarbamates (PNMCs) were considered. Reversed-phase LC was set up for UV and mass spectrometry (MS) detection mode. Gradient elution was used, and the mobile phase was composed of acetonitrile and water. UV-vis was performed at 220 nm. The method was tested with different reversed-phase columns. Comparison between chromatographic parameters: retention time (t R ), resolution (R S ), and selectivity (α) was established. Hydrolysis kinetics of three of the PNMCs were reported. The major hydrolysis products were determined by LC-UV, and the effect of pH on hydrolysis was also studied. Also, chromatographic separation of a mixture of PNMCs and four of their hydrolysis products was carried out. The preconcentration of 12 studied solutes was realized by solid-phase extraction. C18 extraction cartridges of 1 g were used to extract solutes from a 100 mL volume of tap and surface water spiked at 10 μg/L. The recoveries were, respectively, between 68-86% and 62-83% with relative a standard deviation of less than 11%. Limits of detection (LODs) and limits of quantitation (LOQs) ranged, respectively, from 1-4 μg/L and from 4-10 μg/L. Since standard UV detection does not provide adequate selectivity for water samples, an electrospray (ES)-MS instrument equipped with a triple quadrupole mass filter was used. MS data acquisition was performed by a time-scheduled, selected-ion monitoring (SIM) program. Limits of quantitation gave values between 0.1-0.5 μg/L. (author)

Discontinuous structural phase transition of liquid metal and alloys (2)

International Nuclear Information System (INIS)

Wang, Li; Liu, Jiantong

2004-01-01

The diameter (d f ) of diffusion fluid cluster before and after phase transition has been calculated in terms of the paper ''Discontinuous structural phase transition of liquid metal and alloy (1)'' Physics Letters. A 326 (2004) 429-435, to verify quantitatively the discontinuity of structural phase transition; the phenomena of thermal contraction and thermal expansion during the phase transition, together with the evolution model of discontinuous structural phase transition are also discussed in this Letter to explore further the nature of structural transition; In addition, based on the viscosity experimental result mentioned in paper [Y. Waseda, The Structure of Non-Crystalline Materials--Liquids and Amorphous Solids, McGraw-Hill, New York, 1980], we present an approach to draw an embryo of the liquid-liquid (L-L) phase diagram for binary alloys above liquidus in the paper, expecting to guide metallurgy process so as to improve the properties of alloys. The idea that controls amorphous structure and its properties by means of the L-L phase diagram for alloys and by the rapid cooling technique to form the amorphous alloy has been brought forward in the end

Development and validation of a rapid reversed-phase HPLC method for the determination of the non-nucleoside reverse transcriptase inhibitor dapivirine from polymeric nanoparticles.

Science.gov (United States)

das Neves, José; Sarmento, Bruno; Amiji, Mansoor M; Bahia, Maria Fernanda

2010-06-05

The objective of this work was to develop and validate a rapid reversed-phase (RP) high-performance liquid chromatography (HPLC) method for the in vitro pharmaceutical characterization of dapivirine-loaded polymeric nanoparticles. Chromatographic runs were performed on a RP C18 column with a mobile phase comprising acetonitrile-0.5% (w/v) triethanolamine solution in isocratic mode (80:20, v/v) at a flow rate of 1 ml/min. Dapivirine was detected at a wavelength of 290 nm. The method was shown to be specific, linear in the range of 1-50 microg/ml (R(2)=0.9998), precise at the intra-day and inter-day levels as reflected by the relative standard deviation values (less than 0.85%), accurate (recovery rate of 100.17+/-0.35%), and robust to changes in the mobile phase and column brand. The detection and quantitation limits were 0.08 and 0.24 microg/ml, respectively. The method was successfully used to determine the loading capacity and association efficiency of dapivirine in poly(lactic-co-glycolic acid)-based nanoparticles and its in vitro release. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Laser-induced partial oxidation of cyclohexane in liquid phase

International Nuclear Information System (INIS)

Oshima, Y.; Wu, X.W.; Koda, S.

1995-01-01

A laser-induced partial oxidation of cyclohexane was studied in the liquid phase. With KrF excimer laser (248 nm) irradiation to neat liquid cyclohexane in which O 2 was dissolved, cyclohexanol and cyclohexanone were obtained with very high selectivities, together with cyclohexane as a minor product. Radical recombination reactions to produce dicyclohexyl ether and bicyclohexyl also took place, while these products were not observed in the gas phase reaction. These experimental results were considered to be due not only to higher concentration of cyclohexane but to the cage effect in the liquid phase oxidation. To clarify the reaction progress including the photoabsorption process, the effects of laser intensity and O 2 pressure on product distribution were studied. (author)

[Application of off-line two dimensional reversed-phase liquid chromatography/supercritical fluid chromatography to the separation of the seeds of Trichosanthes kirilowii Maxim].

Science.gov (United States)

Yuan, Yun; Xin, Huaxia; Peng, Ziyue; Fu, Qing; Jin, Yu

2017-07-08

An off-line two dimensional reversed-phase liquid chromatography/supercritical fluid chromatography (2D RPLC/SFC) method was developed for the separation of the seeds of Trichosanthes kirilowii Maxim . ( T. kirilowii .). In the experiment, RPLC was used in the first dimension to analyze the samples. And 12 fractions (F 1 -F 12 ) were obtained according to the chromatographic peak collection mode, the fractions were re-analyzed in both RPLC and SFC modes. The results clearly showed that this 2D method had good orthogonality. The SFC was used as the second dimension. Ethanol- n -hexane (3:7, v/v) was used as a modifier in SFC. The modifier could provide appropriate elution power. When the sample load increased, it could also ensure the solubility of samples. The 2D RPLC/SFC method had obvious advantages for separating the compounds with similar properties, enriching and purifying the trace components. Finally, 150 peaks could be detected. The off-line 2D RPLC/SFC method will be further enlarged to a preparative level for preparation of compounds. The method can provide a practical reference for the purification of chemical constituents and material basis research of the seeds of T. kirilowii . in the future.

Liquid phase sintered superconducting cermet

International Nuclear Information System (INIS)

Ray, S.P.

1990-01-01

This patent describes a method of making a superconducting cermet having superconducting properties with improved bulk density, low porosity and in situ stabilization. It comprises: forming a structure of a superconducting ceramic material having the formula RM 2 Cu 3 O (6.5 + x) wherein R is one or more rare earth elements capable of reacting to form a superconducting ceramic, M is one or more alkaline earth metal elements selected from barium and strontium capable of reacting to form a superconducting ceramic, x is greater than 0 and less than 0.5; and a precious metal compound in solid form selected from the class consisting of oxides, sulfides and halides of silver; and liquid phase sintering the mixture at a temperature wherein the precious metal of the precious metal compound is molten and below the melting point of the ceramic material. The liquid phase sintering is carried out for a time less than 36 hours but sufficient to improve the bulk density of the cermet

Highly tilted liquid crystalline materials possessing a direct phase transition from antiferroelectric to isotropic phase

Energy Technology Data Exchange (ETDEWEB)

Milewska, K.; Drzewiński, W. [Institute of Chemistry, Military University of Technology, 00-908 Warsaw (Poland); Czerwiński, M., E-mail: mczerwinski@wat.edu.pl [Institute of Chemistry, Military University of Technology, 00-908 Warsaw (Poland); Dąbrowski, R. [Institute of Chemistry, Military University of Technology, 00-908 Warsaw (Poland); Piecek, W. [Institute of Applied Physics, Military University of Technology, 00-908 Warsaw (Poland)

2016-03-01

Pure compounds and multicomponent mixtures with a broad temperature range of high tilted liquid crystalline antiferroelectric phase and a direct phase transition from antiferroelectric to isotropic phase, were obtained. X-ray diffraction analysis confirms these kinds of materials form a high tilted anticlinic phase, with a fixed layer spacing and very weak dependency upon temperature, after the transition from the isotropic phase. Due to this, not only pure orthoconic antiferroelectric liquid crystals but also those with a moderate tilt should generate a good dark state. Furthermore, due to the increased potential for forming anticlinic forces, such materials could minimize a commonly observed asymmetry of a rise and fall switching times at a surface stabilized geometry. - Highlights: • The new class of liquid crystalline materials with the direct SmC{sub A}*. • Iso phase transition were obtained. • Materials possess the layer spacing fixed and very weak dependent upon temperature. • Smectic layers without shrinkage are observed. • A good dark state can be generate in SSAFLC.

Carbon nanoparticle stabilised liquid|liquid micro-interfaces for electrochemically driven ion-transfer processes

International Nuclear Information System (INIS)

MacDonald, Stuart M.; Fletcher, Paul D.I.; Cui Zhenggang; Opallo, Marcin; Chen Jingyuan; Marken, Frank

2007-01-01

Stabilised liquid|liquid interfaces between an organic 4-(3-phenylpropyl)-pyridine (PPP) phase and an aqueous electrolyte phase are obtained in the presence of suitable nanoparticles. The use of nanoparticulate stabilisers (ca. 30 nm diameter laponite or 9-18 nm diameter carbon) in 'Pickering' emulsion systems allows stable organic microdroplets to be formed and these are readily deposited onto conventional tin-doped indium oxide (ITO) electrodes. In contrast to the electrically insulating laponite nanoparticles, conducting carbon nanoparticles are shown to effectively catalyse the simultaneous electron transfer and ion transfer process at triple phase boundary junctions. Anion transfer processes between the aqueous and organic phase are driven electrochemically at the extensive triple phase junction carbon nanoparticle|4-(3-phenylpropyl)-pyridine|aqueous electrolyte. The organic phase consists of a redox active reagent 5,10,15,20-tetraphenyl-21H,23H-porphinato manganese(III) (MnTPP + ), 5,10,15,20-tetraphenyl-21H,23H-porphinato iron(III) (FeTPP + ), or proto-porphyrinato-IX iron(III) (hemin) dissolved in 4-(3-phenylpropyl)-pyridine (PPP). The composition of the aqueous electrolyte phase determines the reversible potential for the Nernstian anion transfer process. The methodology is shown to be versatile and, in future, could be applied more generally in liquid|liquid electroanalysis

Three-dimensionally Functionalized Reverse Phase Glycoprotein Array for Cancer Biomarker Discovery and Validation

OpenAIRE

Pan, Li; Aguilar, Hillary Andaluz; Wang, Linna; Iliuk, Anton; Tao, W. Andy

2016-01-01

Glycoproteins have vast structural diversity which plays an important role in many biological processes and have great potential as disease biomarkers. Here we report a novel functionalized reverse phase protein array (RPPA), termed polymer-based reverse phase GlycoProtein Array (polyGPA), to specifically capture and profile glycoproteomes, and validate glycoproteins. Nitrocellulose membrane functionalized with globular hydroxyaminodendrimers was used to covalently capture pre-oxidized glycan...

Chromatographic retention prediction and octanol-water partition coefficient determination of monobasic weak acidic compounds in ion-suppression reversed-phase liquid chromatography using acids as ion-suppressors.

Science.gov (United States)

Ming, Xin; Han, Shu-ying; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

2009-08-15

Although simple acids, replacing buffers, have been widely applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography (RPLC), none of the previously reported works focused on the systematic studies about the retention behavior of the acidic solutes in this ion-suppression RPLC mode. The subject of this paper was therefore to investigate the retention behavior of monobasic weak acidic compounds using acetic, perchloric and phosphoric acids as the ion-suppressors. The apparent octanol-water partition coefficient (K" ow) was proposed to calibrate the octanol-water partition coefficient (K(ow)) of these weak acidic compounds, which resulted in a better linear correlation with log k(w), the logarithm of the hypothetical retention factor corresponding to neat aqueous fraction of hydroorganic mobile phase. This log K" ow-log k w linear correlation was successfully validated by the results of monocarboxylic acids and monohydrating phenols, and moreover by the results under diverse experimental conditions for the same solutes. This straightforward relationship not only can be used to effectively predict the retention values of weak acidic solutes combined with Snyder-Soczewinski equation, but also can offer a promising medium for directly measuring K(ow) data of these compounds via Collander equation. In addition, the influence of the different ion-suppressors on the retention of weak acidic compounds was also compared in this RPLC mode.

The liquid to vapor phase transition in excited nuclei

Energy Technology Data Exchange (ETDEWEB)

Elliott, J.B.; Moretto, L.G.; Phair, L.; Wozniak, G.J.; Beaulieu, L.; Breuer, H.; Korteling, R.G.; Kwiatkowski, K.; Lefort, T.; Pienkowski, L.; Ruangma, A.; Viola, V.E.; Yennello, S.J.

2001-05-08

For many years it has been speculated that excited nuclei would undergo a liquid to vapor phase transition. For even longer, it has been known that clusterization in a vapor carries direct information on the liquid-vapor equilibrium according to Fisher's droplet model. Now the thermal component of the 8 GeV/c pion + 197 Au multifragmentation data of the ISiS Collaboration is shown to follow the scaling predicted by Fisher's model, thus providing the strongest evidence yet of the liquid to vapor phase transition.

Liquid Crystals - The 'Fourth' Phase of Matter

Indian Academy of Sciences (India)

possibilities of novel technological applications. Liquid crystalline materials ... advanced instrumentation, including laptops and futuristic flat panel displays. .... The twist grain-boundary phase is formed when the layers of a smectic A phase are .... the optic axis) is uniformly oriented parallel to the glass plate. (see Figure IIa).

Plasmas in Multiphase Media: Bubble Enhanced Discharges in Liquids and Plasma/Liquid Phase Boundaries

Energy Technology Data Exchange (ETDEWEB)

Kushner, Mark Jay [University of Michigan

2014-07-10

In this research project, the interaction of atmospheric pressure plasmas with multi-phase media was computationally investigated. Multi-phase media includes liquids, particles, complex materials and porous surfaces. Although this investigation addressed fundamental plasma transport and chemical processes, the outcomes directly and beneficially affected applications including biotechnology, medicine and environmental remediation (e.g., water purification). During this project, we made advances in our understanding of the interaction of atmospheric pressure plasmas in the form of dielectric barrier discharges and plasma jets with organic materials and liquids. We also made advances in our ability to use computer modeling to represent these complex processes. We determined the method that atmospheric pressure plasmas flow along solid and liquid surfaces, and through endoscopic like tubes, deliver optical and high energy ion activation energy to organic and liquid surfaces, and produce reactivity in thin liquid layers, as might cover a wound. We determined the mechanisms whereby plasmas can deliver activation energy to the inside of liquids by sustaining plasmas in bubbles. These findings are important to the advancement of new technology areas such as plasma medicine

Solid-Phase Extraction and Reverse-Phase HPLC: Application to Study the Urinary Excretion Pattern of Benzophenone-3 and its Metabolite 2,4-Dihydroxybenzophenone in Human Urine

Directory of Open Access Journals (Sweden)

Helena Gonzalez

2008-01-01

Full Text Available Background Benzophenone-3 (BZ-3 is a common ultraviolet (UV absorbing compound in sunscreens. It is the most bioavailable species of all UV-absorbing compounds after topical application and can be found in plasma and urine. Objectives The aim of this study was to develop a reverse-phase high performance liquid chromatography (HPLC method for determining the amounts BZ-3 and its metabolite 2,4-dihydroxybenzophenone (DHB in human urine. The method had to be suitable for handling a large number of samples. It also had to be rapid and simple, but still sensitive, accurate and reproducible. The assay was applied to study the urinary excretion pattern after repeated whole-body applications of a commercial sunscreen, containing 4% BZ-3, to 25 healthy volunteers. Methods Each sample was analyzed with regard to both conjugated/non-conjugated BZ-3 and conjugated/non-conjugated DHB, since both BZ-3 and DHB are extensively conjugated in the body. Solid-phase extraction (SPE with C8 columns was followed by reverse-phase HPLC. For separation a Genesis C18 column was used with an acethonitrile-water mobile phase and the UV-detector was set at 287 nm. Results The assay was linear r 2 > 0.99, with detection limits for BZ-3 and DHB of 0.01 µmol L -1 and 0.16 µmol L -1 respectively. Relative standard deviation (RSD was less than 10% for BZ-3 and less than 13% for DHB. The excretion pattern varied among the human volunteers; we discerned different patterns among the individuals. Conclusions The reverse-phase HPLC assay and extraction procedures developed are suitable for use when a large number of samples need to be analyzed and the method fulfilled our objectives. The differences in excretion pattern may be due to differences in enzyme activity but further studies, especially about genetic polymorphism, need to be performed to verify this finding.

Determination of NVP-BEZ235, a dual PI3K and mTOR inhibitor, in human and mouse plasma and in mouse tissue homogenates by reversed-phase high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Lin, Fan; Chandrasekaran, Gayathri; de Gooijer, Mark C; Beijnen, Jos H; van Tellingen, Olaf

2012-07-15

NVP-BEZ235 is a novel dual inhibitor of PI3K/mTOR and currently undergoing phase I/II clinical trials for advanced solid tumors. We developed a sensitive and selective reversed-phase high-performance liquid chromatographic (HPLC) assay with fluorometric detection for quantification of NVP-BEZ235 in biological matrices. Liquid-liquid extraction with tert-butyl methyl ether was used for sample pre-treatment, yielding a recovery of >84%. Chromatographic separation of NVP-BEZ235 and the internal standard (IS) NVP-BBD130 was achieved on a GraceSmart C-18 column by isocratic elution with a mobile phase which consisted of acetonitrile, methanol, and milliQ water adjusted with acetic acid to pH 3.7 (20:36:44, v/v/v). Fluorescence detection using excitation and emission wavelengths of 270 and 425 nm, respectively, provided a selectivity and sensitivity allowing quantification down to 1 ng/ml in human plasma and linear calibration curves within a range of 1-1000 ng/ml. The assay was validated for human plasma, mouse plasma and a range of tissues. The accuracy, within-day and between-day precision for all matrices, was within the generally accepted 15% range. NVP-BEZ235 was stable for 72 h in pretreated samples in reconstitution mixture (acetonitrile-water (30:70, v/v)), but unstable in mouse tissue homogenates upon repeated freeze-thaw cycles or long term storage (≥24 h) at room temperature. A pilot pharmacokinetic study in mice demonstrated the applicability of this method for pharmacokinetic purposes. Overall, this assay is suitable for the pharmacokinetic studies of NVP-BEZ235 in mice and in human plasma. Copyright © 2012 Elsevier B.V. All rights reserved.

Characterisation of GERDA Phase-I detectors in liquid argon

Energy Technology Data Exchange (ETDEWEB)

Barnabe Heider, Marik; Schoenert, Stefan [Max-Planck-Institut fuer Kernphysik (Germany); Gusev, Konstantin [Russian Research Center, Kurchatov Institute (Russian Federation); Joint Institute for Nuclear Research (Russian Federation)

2009-07-01

GERDA will search for neutrinoless double beta decay in {sup 76}Ge by submerging bare enriched HPGe detectors in liquid argon. In GERDA Phase-I, reprocessed enriched-Ge detectors, which were previously operated by the Heidelberg-Moscow and IGEX collaborations, and reprocessed natural-Ge detectors from Genius-TF, will be redeployed. We have tested the operation and performance of bare HPGe detectors in liquid nitrogen and in liquid argon over more than three years with three non-enriched p-type prototype detectors. The detector handling and mounting procedures have been defined and the Phase-I detector technology, the low-mass assembly and the long-term stability in liquid argon have been tested successfully. The Phase-I detectors were reprocessed by Canberra Semiconductor NV, Olen, according to their standard technology but without the evaporation of a passivation layer. After their reprocessing, the detectors have been mounted in their low-mass holders and their characterisation in liquid argon performed. The leakage current, the counting characteristics and the efficiency of the detectors have been measured. The testing of the detectors was carried out in the liquid argon test stand of the GERDA underground Detector Laboratory (GDL) at LNGS. The detectors are now stored underground under vacuum until their operation in GERDA.

Reversed-Phase UHPLC Enantiomeric Separation of Rasagiline Salts Using a Chiralpak® AGP Column

Directory of Open Access Journals (Sweden)

Nagarajan Balaji

2017-07-01

Full Text Available We report the first rapid ultra-high performance liquid chromatographic (UHPLC enantiomeric reversed-phase separation of rasagiline mesylate and its tartrate salts using a Chiralpak® AGP column (50 mm × 2.1 mm, 5 μm as a stationary phase. This method was developed as an alternative to the usage of previously reported normal-phase chiral LC columns for isomer separation. Our method is based on an isocratic approach using a mixture of ammonium acetate and isopropyl alcohol (90:10, v/v as the mobile phase (0.6 mL/min flow rate. The detection limit (at a detection wavelength of 210 nm and quantification limit for the rasagiline enantiomers were 0.06 and 0.2 μg/mL, respectively. This method is compatible with the UHPLC-MS technique. The successful separation of rasagiline and its enantiomer was confirmed by determining the corresponding specific optical rotation values. Our method will be applicable for detecting rasagiline enantiomers during the control of manufacturing processes, and for use in rapid analysis for quality control in pharmaceutical industry to obtain optically pure pharmaceutical substances. This method was validated in terms of its precision, limit of detection, limit of quantification, linearity, accuracy, robustness, ruggedness, specificity, forced degradation, and solution stability, according to International Council on Harmonization Validation Guidelines Q2 (R1.

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.)

Origins of phase contrast in the atomic force microscope in liquids

OpenAIRE

Melcher, John; Carrasco, Carolina; Xu, Xianfan; Carrascosa, Jose L; Gomez-Herrero, Julio; Jose de Pablo, Pedro; Raman, Arvind

2009-01-01

We study the physical origins of phase contrast in dynamic atomic force microscopy (dAFM) in liquids where low-stiffness microcantilever probes are often used for nanoscale imaging of soft biological samples with gentle forces. Under these conditions, we show that the phase contrast derives primarily from a unique energy flow channel that opens up in liquids due to the momentary excitation of higher eigenmodes. Contrary to the common assumption, phase-contrast images in liquids using soft mic...

Comparison of Various Types of Stationary Phases in Non-Aqueous Reversed-Phase High-Performance Liquid Chromatography–Mass Spectrometry of Glycerolipids in Blackcurrant Oil and Its Enzymatic Hydrolysis Mixture

Czech Academy of Sciences Publication Activity Database

Lísa, M.; Holčapek, M.; Sovová, Helena

2009-01-01

Roč. 1216, č. 47 (2009), s. 8371-8378 ISSN 0021-9673 Institutional research plan: CEZ:AV0Z40720504 Keywords : ultra high-performance liquid chromatography * C30 stationary phase * triacylglycerols Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.101, year: 2009

Computation of liquid-liquid equilibria and phase stabilities: implications for RH-dependent gas/particle partitioning of organic-inorganic aerosols

Directory of Open Access Journals (Sweden)

A. Zuend

2010-08-01

Full Text Available Semivolatile organic and inorganic aerosol species partition between the gas and aerosol particle phases to maintain thermodynamic equilibrium. Liquid-liquid phase separation into an organic-rich and an aqueous electrolyte phase can occur in the aerosol as a result of the salting-out effect. Such liquid-liquid equilibria (LLE affect the gas/particle partitioning of the different semivolatile compounds and might significantly alter both particle mass and composition as compared to a one-phase particle. We present a new liquid-liquid equilibrium and gas/particle partitioning model, using as a basis the group-contribution model AIOMFAC (Zuend et al., 2008. This model allows the reliable computation of the liquid-liquid coexistence curve (binodal, corresponding tie-lines, the limit of stability/metastability (spinodal, and further thermodynamic properties of multicomponent systems. Calculations for ternary and multicomponent alcohol/polyol-water-salt mixtures suggest that LLE are a prevalent feature of organic-inorganic aerosol systems. A six-component polyol-water-ammonium sulphate system is used to simulate effects of relative humidity (RH and the presence of liquid-liquid phase separation on the gas/particle partitioning. RH, salt concentration, and hydrophilicity (water-solubility are identified as key features in defining the region of a miscibility gap and govern the extent to which compound partitioning is affected by changes in RH. The model predicts that liquid-liquid phase separation can lead to either an increase or decrease in total particulate mass, depending on the overall composition of a system and the particle water content, which is related to the hydrophilicity of the different organic and inorganic compounds. Neglecting non-ideality and liquid-liquid phase separations by assuming an ideal mixture leads to an overestimation of the total particulate mass by up to 30% for the composition and RH range considered in the six

Simultaneous determination of Cr(iii) and Cr(vi) using reversed-phased ion-pairing liquid chromatography with dynamic reaction cell inductively coupled plasma mass spectrometry

Science.gov (United States)

Wolf, R.E.; Morrison, J.M.; Goldhaber, M.B.

2007-01-01

A method for the simultaneous determination of Cr(iii) and Cr(vi) species in waters, soil leachates and synthetic bio-fluids is described. The method uses reversed-phase ion-pairing liquid chromatography to separate the chromium species and a dynamic reaction cell (DRC??) equipped ICP-MS for detection of chromium. Separation of the chromium species is carried out in less than 2 min. Cr(iii) is complexed with ethylenediaminetetraacetic acid (EDTA) prior to separation by mixing samples with the mobile phase containing 2.0 mM tetrabutylammonium hydroxide (TBAOH), 0.5 mM EDTA (dipotassium salt), and 5% (vol/vol) methanol, adjusted to pH 7.6. The interfering 40Ar 12C+ background peak at mass 52 was reduced by over four orders of magnitude to less than 200 cps by using 0.65 mL min-1 ammonia as a reaction gas and an RPq setting on the DRC of 0.75. Method detection limits (MDLs) of 0.09 ??g L-1 for Cr(iii) and 0.06 ??g L-1 for Cr(vi) were obtained based on peak areas at mass 52 for 50 ??L injections of low level spikes. Reproducibility at 2 ??g L-1 was 3% RSD for 5 replicate injections. The tolerance of the method to various levels of common cations and anions found in natural waters and to matrix constituents found in soil leachates and simulated gastric and lung fluids was tested by performing spike recovery calculations for a variety of samples. ?? The Royal Society of Chemistry.

Metastable liquid-liquid transition in a molecular model of water

Science.gov (United States)

Palmer, Jeremy C.; Martelli, Fausto; Liu, Yang; Car, Roberto; Panagiotopoulos, Athanassios Z.; Debenedetti, Pablo G.

2014-06-01

Liquid water's isothermal compressibility and isobaric heat capacity, and the magnitude of its thermal expansion coefficient, increase sharply on cooling below the equilibrium freezing point. Many experimental, theoretical and computational studies have sought to understand the molecular origin and implications of this anomalous behaviour. Of the different theoretical scenarios put forward, one posits the existence of a first-order phase transition that involves two forms of liquid water and terminates at a critical point located at deeply supercooled conditions. Some experimental evidence is consistent with this hypothesis, but no definitive proof of a liquid-liquid transition in water has been obtained to date: rapid ice crystallization has so far prevented decisive measurements on deeply supercooled water, although this challenge has been overcome recently. Computer simulations are therefore crucial for exploring water's structure and behaviour in this regime, and have shown that some water models exhibit liquid-liquid transitions and others do not. However, recent work has argued that the liquid-liquid transition has been mistakenly interpreted, and is in fact a liquid-crystal transition in all atomistic models of water. Here we show, by studying the liquid-liquid transition in the ST2 model of water with the use of six advanced sampling methods to compute the free-energy surface, that two metastable liquid phases and a stable crystal phase exist at the same deeply supercooled thermodynamic condition, and that the transition between the two liquids satisfies the thermodynamic criteria of a first-order transition. We follow the rearrangement of water's coordination shell and topological ring structure along a thermodynamically reversible path from the low-density liquid to cubic ice. We also show that the system fluctuates freely between the two liquid phases rather than crystallizing. These findings provide unambiguous evidence for a liquid-liquid transition in

Simultaneous determination of linagliptin and metformin by reverse phase-high performance liquid chromatography method: An application in quantitative analysis of pharmaceutical dosage forms

Directory of Open Access Journals (Sweden)

Prathyusha Vemula

2015-01-01

Full Text Available To enhance patient compliance toward treatment in diseases like diabetes, usually a combination of drugs is prescribed. Therefore, an anti-diabetic fixed-dose combination of 2.5 mg of linagliptin 500 mg of metformin was taken for simultaneous estimation of both the drugs by reverse phase-high performance liquid chromatography (RP-HPLC method. The present study aimed to develop a simple and sensitive RP-HPLC method for the simultaneous determination of linagliptin and metformin in pharmaceutical dosage forms. The chromatographic separation was designed and evaluated by using linagliptin and metformin working standard and sample solutions in the linearity range. Chromatographic separation was performed on a C 18 column using a mobile phase of 70:30 (v/v mixture of methanol and 0.05 M potassium dihydrogen orthophosphate (pH adjusted to 4.6 with orthophosphoric acid delivered at a flow rate of 0.6 mL/min and UV detection at 267 nm. Linagliptin and metformin shown linearity in the range of 2-12 μg/mL and 400-2400 μg/mL respectively with correlation co-efficient of 0.9996 and 0.9989. The resultant findings analyzed for standard deviation (SD and relative standard deviation to validate the developed method. The retention time of linagliptin and metformin was found to be 6.3 and 4.6 min and separation was complete in <10 min. The method was validated for linearity, accuracy and precision were found to be acceptable over the linearity range of the linagliptin and metformin. The method was found suitable for the routine quantitative analysis of linagliptin and metformin in pharmaceutical dosage forms.

Determination of Letrozole in Tablet Formulations by Reversed ...

African Journals Online (AJOL)

Determination of Letrozole in Tablet Formulations by Reversed Phase High Performance Liquid Chromatography. ... The assay values for the two branded letrozole tablets tested were 99.2 and 100.2 %, respectively with % relative standard deviation (RSD) of 0.781 and 0.568, respectively. The bench top stability data of the ...

Spatial heterogeneity in liquid–liquid phase transition

International Nuclear Information System (INIS)

Duan Yun-Rui; Li Tao; Wu Wei-Kang; Li Jie; Zhou Xu-Yan; Liu Si-Da; Li Hui

2017-01-01

Molecular dynamics simulations are performed to investigate the liquid–liquid phase transition (LLPT) and the spatial heterogeneity in Al–Pb monotectic alloys. The results reveal that homogeneous liquid Al–Pb alloy undergoes an LLPT, separating into Al-rich and Pb-rich domains, which is quite different from the isocompositional liquid water with a transition between low-density liquid (LDL) and high-density liquid (HDL). With spatial heterogeneity becoming large, LLPT takes place correspondingly. The relationship between the cooling rate, relaxation temperature and percentage of Al and the spatial heterogeneity is also reported. This study may throw light on the relationship between the structure heterogeneity and LLPT, which provides novel strategies to control the microstructures in the fabrication of the material with high performance. (paper)

Not spreading in reverse: The dewetting of a liquid film into a single drop.

Science.gov (United States)

Edwards, Andrew M J; Ledesma-Aguilar, Rodrigo; Newton, Michael I; Brown, Carl V; McHale, Glen

2016-09-01

Wetting and dewetting are both fundamental modes of motion of liquids on solid surfaces. They are critically important for processes in biology, chemistry, and engineering, such as drying, coating, and lubrication. However, recent progress in wetting, which has led to new fields such as superhydrophobicity and liquid marbles, has not been matched by dewetting. A significant problem has been the inability to study the model system of a uniform film dewetting from a nonwetting surface to a single macroscopic droplet-a barrier that does not exist for the reverse wetting process of a droplet spreading into a film. We report the dewetting of a dielectrophoresis-induced film into a single equilibrium droplet. The emergent picture of the full dewetting dynamics is of an initial regime, where a liquid rim recedes at constant speed and constant dynamic contact angle, followed by a relatively short exponential relaxation of a spherical cap shape. This sharply contrasts with the reverse wetting process, where a spreading droplet follows a smooth sequence of spherical cap shapes. Complementary numerical simulations and a hydrodynamic model reveal a local dewetting mechanism driven by the equilibrium contact angle, where contact line slip dominates the dewetting dynamics. Our conclusions can be used to understand a wide variety of processes involving liquid dewetting, such as drop rebound, condensation, and evaporation. In overcoming the barrier to studying single film-to-droplet dewetting, our results provide new approaches to fluid manipulation and uses of dewetting, such as inducing films of prescribed initial shapes and slip-controlled liquid retraction.

Laser-induced microscopic phase-transition on an ionic liquid

International Nuclear Information System (INIS)

Iguchi, Natsuki; Datta, Alokmay; Yoshikawa, Kenichi; Ma Yue

2009-01-01

Nematic-isotropic transition is induced in a 5 μm 'droplet' within an oriented bulk of a mixture of a liquid crystalline material with a room-temperature ionic liquid, by a laser working at 532 nm with an output power of 200 mW and a beam diameter of 1 μm. No microscopic phase transition is observed either in absence of the ionic liquid or at the other wavelength of 1064 nm, available to the Nd-YAG laser. This indicates the essential role on a resonant transfer of energy to the ionic liquid from the laser radiation, which is subsequently transferred to the liquid crystal. Spectroscopy of the pure liquid crystal and ionic liquid samples confirms this concept. Spatio-temporal image of the droplet growth shows, however, that the phase transition remains confined within the microscopic domain for the first 50 s, and then spreads out rapidly. Since resonant, quantum transitions between molecular levels takes place in less than microseconds, the about seven orders of magnitude slowing down of energy transfer observed here suggests unique hierarchical dynamics including the coupling between the intra-molecular motions in the ionic liquid and the inter-molecular forces between ionic liquid and liquid crystal.

Ion-pairing reversed-phased chromatography/mass spectrometry of heparin

DEFF Research Database (Denmark)

Henriksen, Jens; Roepstorff, Peter; Ringborg, Lene H.

2006-01-01

not well characterised. In order to further characterise such mixtures, two on-line ion-pairing reverse-phased chromatography electrospray ionisation (ESI) mass spectrometry methods have been developed. One of the systems allows the determination of more than 200 components in a medium molecular weight...

Reverse capillary flow of condensed water through aligned multiwalled carbon nanotubes

International Nuclear Information System (INIS)

Yun, Jongju; Jeon, Wonjae; Alam Khan, Fakhre; Lee, Jinkee; Baik, Seunghyun

2015-01-01

Molecular transport through nanopores has recently received considerable attention as a result of advances in nanofabrication and nanomaterial synthesis technologies. Surprisingly, water transport investigations through carbon nanochannels resulted in two contradicting observations: extremely fast transport or rejection of water molecules. In this paper, we elucidate the mechanism of impeded water vapor transport through the interstitial space of aligned multiwalled carbon nanotubes (aligned-MWCNTs)—capillary condensation, agglomeration, reverse capillary flow, and removal by superhydrophobicity at the tip of the nanotubes. The origin of separation comes from the water’s phase change from gas to liquid, followed by reverse capillary flow. First, the saturation water vapor pressure is decreased in a confined space, which is favorable for the phase change of incoming water vapor into liquid drops. Once continuous water meniscus is formed between the nanotubes by the adsoprtion and agglomeration of water molecules, a high reverse Laplace pressure is induced in the mushroom-shaped liquid meniscus at the entry region of the aligned-MWCNTs. The reverse Laplace pressure can be significantly enhanced by decreasing the pore size. Finally, the droplets pushed backward by the reverse Laplace pressure can be removed by superhydrophobicity at the tip of the aligned-MWCNTs. The analytical analysis was also supported by experiments carried out using 4 mm-long aligned-MWCNTs with different intertube distances. The water rejection rate and the separation factor increased as the intertube distance decreased, resulting in 90% and 10, respectively, at an intertube distance of 4 nm. This mechanism and nanotube membrane may be useful for energy-efficient water vapor separation and dehumidification. (paper)

Determination of mycophenolic acid in mest products using mixed mode reversed phase-anion exchange clean-up and liquid chromatography-high-resolution mass spectrometry

DEFF Research Database (Denmark)

Sørensen, Louise Marie; Nielsen, Kristian Fog; Jacobsen, Thomas

2008-01-01

A method for determination of mycophenolic acid (MPA) in dry-cured ham, fermented sausage and liver pate is described. MPA was extracted from meat with bicarbonate-acetonitrile, further cleaned-up by mixed mode reversed phase-anion exchange and detected using a LC-MS system with electrospray...

The liquid protein phase in crystallization: a case study—intact immunoglobulins

Science.gov (United States)

Kuznetsov, Yurii G.; Malkin, Alexander J.; McPherson, Alexander

2001-11-01

A common observation by protein chemists has been the appearance, for many proteins in aqueous solutions, of oil like droplets, or in more extreme cases the formation of a second oil like phase. These may accompany the formation of precipitate in "salting out" or "salting in' procedures, but more commonly appear in place of any precipitate. Such phase separations also occur, with even greater frequency, in the presence of polymeric precipitants such as polyethyleneglycol (PEG). In general the appearance of a second liquid phase has been taken as indicative of protein aggregation, though an aggregate state distinctly different from that characteristic of amorphous precipitate. While the latter is thought to be composed of linear and branched assemblies, polymers of a sort, the oil phase suggests a more compact, three-dimensional, but fluid state. An important property of an alternate, fluid phase is that it can mediate transitions between other states, for example, between protein molecules free in solution and protein molecules immobilized in amorphous precipitate or crystals. The "liquid protein" phase can be readily observed in many crystallization experiments either prior to the appearance of visible crystals, or directly participating in the crystal growth process. In some cases the relationship between the liquid phase and developing crystals is intimate. Crystals grow directly from the liquid phase, or appear only after the visible formation of the liquid phase. We describe here our experience with a class of macromolecules, immunoglobulins, and particularly IDEC-151, an IgG specific for CD4 on human lymphocytes. This protein has been crystallized from a Jeffamine-LiSO 4 mother liquor and, its crystallization illustrates many of the features associated with the liquid protein, or protein rich phase.

Cone-shaped membrane liquid phase micro extraction

International Nuclear Information System (INIS)

Hong, Heng See; Sanagi, M.M.; Ibrahim, W.A.W.; Naim, A.A.

2008-01-01

A novel sample pre-treatment technique termed cone-shaped membrane liquid phase micro extraction (CSM-LPME) was developed and combined with micro-liquid chromatography (micro-LC) for the determination of selected pesticides in water samples. Several important extraction parameters such as types of extraction solvent, agitation rate, pH value, total exposure time and effect of salt and humic acids were investigated and optimized. Enrichment factors of >50 folds were easily achieved within 20 min of extraction. The new developed method demonstrated an excellent performance in terms of speed, cost effectiveness, reproducibility, as well as exceptional low detection limits. Current work provides a great interest to further investigate on the applicability of the CSM-LPME technique in analytical chemistry and explores the possibility of replacing conventional extraction techniques such as soxhlet, solid phase extraction (SPE) and solid phase micro extraction (SPME). (author)

Glass phase expelling during liquid phase sintering of YSZ

International Nuclear Information System (INIS)

Souza, Milton Ferreira de; Souza, Dulcina Pinatti Ferreira de

1998-01-01

Expelling of the liquid phase during sintering of Zr O 2 -6.5 mol % Y 2 O 3 - 0.5 mol % Pr 2 O 3 ceramic was observed as a result of grain coarsening. ZrO 2 - 7.0 mol % Y 2 O 3 samples, without Pr 2 O 3 addition, do not show this effect under the same sintering conditions. The expelling process is caused by surface tension forces and attracting van der Waals forces between the grains, coupled with the existence of two glass phases on the grain boundaries. The amount of expelled glass phase increases with grain growth, but saturates above 16 μm average grain size. (author)

Local gas- and liquid-phase measurements for air-water two-phase flows in a rectangular channel

International Nuclear Information System (INIS)

Zhou, X.; Sun, X.; Williams, M.; Fu, Y.; Liu, Y.

2014-01-01

Local gas- and liquid-phase measurements of various gas-liquid two-phase flows, including bubbly, cap-bubbly, slug, and churn-turbulent flows, were performed in an acrylic vertical channel with a rectangular cross section of 30 mm x 10 mm and height of 3.0 m. All the measurements were carried out at three measurement elevations along the flow channel, with z/D h = 9, 72, and 136, respectively, to study the flow development. The gas-phase velocity, void fraction, and bubble number frequency were measured using a double-sensor conductivity probe. A high-speed imaging system was utilized to perform the flow regime visualization and to provide additional quantitative information of the two-phase flow structure. An image processing scheme was developed to obtain the gas-phase velocity, void fraction, Sauter mean diameter, bubble number density, and interfacial area concentration. The liquid-phase velocity and turbulence measurements were conducted using a particle image velocimetry-planar laser-induced fluorescence (PIV-PLIF) system, which enables whole-field and high-resolution data acquisition. An optical phase separation method, which uses fluorescent particles and optical filtration technique, is adopted to extract the velocity information of the liquid phase. An image pre-processing scheme is imposed on the raw PIV images acquired to remove noises due to the presence of bubble residuals and optically distorted particles in the images captured by the PIV-PLIF system. Due to the better light access and less bubble distortion in the narrow rectangular channel, the PIV-PLIF system were able to perform reasonably well in flows of even higher void fractions as compared to the situations with circular pipe test sections. The flow conditions being studied covered various flow regime transitions, void fractions, and liquid-phase flow Reynolds numbers. The obtained experimental data can also be used to validate two-phase CFD results. (author)

Modeling the gas-particle partitioning of secondary organic aerosol: the importance of liquid-liquid phase separation

Directory of Open Access Journals (Sweden)

A. Zuend

2012-05-01

Full Text Available The partitioning of semivolatile organic compounds between the gas phase and aerosol particles is an important source of secondary organic aerosol (SOA. Gas-particle partitioning of organic and inorganic species is influenced by the physical state and water content of aerosols, and therefore ambient relative humidity (RH, as well as temperature and organic loading levels. We introduce a novel combination of the thermodynamic models AIOMFAC (for liquid mixture non-ideality and EVAPORATION (for pure compound vapor pressures with oxidation product information from the Master Chemical Mechanism (MCM for the computation of gas-particle partitioning of organic compounds and water. The presence and impact of a liquid-liquid phase separation in the condensed phase is calculated as a function of variations in relative humidity, organic loading levels, and associated changes in aerosol composition. We show that a complex system of water, ammonium sulfate, and SOA from the ozonolysis of α-pinene exhibits liquid-liquid phase separation over a wide range of relative humidities (simulated from 30% to 99% RH. Since fully coupled phase separation and gas-particle partitioning calculations are computationally expensive, several simplified model approaches are tested with regard to computational costs and accuracy of predictions compared to the benchmark calculation. It is shown that forcing a liquid one-phase aerosol with or without consideration of non-ideal mixing bears the potential for vastly incorrect partitioning predictions. Assuming an ideal mixture leads to substantial overestimation of the particulate organic mass, by more than 100% at RH values of 80% and by more than 200% at RH values of 95%. Moreover, the simplified one-phase cases stress two key points for accurate gas-particle partitioning calculations: (1 non-ideality in the condensed phase needs to be considered and (2 liquid-liquid phase separation is a consequence of considerable deviations

Structural crossover in a supercooled metallic liquid and the link to a liquid-to-liquid phase transition

Energy Technology Data Exchange (ETDEWEB)

Lan, S.; Ma, J. L.; Fan, J. [Department of Physics and Material Science, City University of Hong Kong 83 Tat Chee Ave., Kowloon (Hong Kong); Blodgett, M.; Kelton, K. F. [Department of Physics and Institute of Materials Science and Engineering, Washington University One Brookings Drive, St. Louis, Missouri 63130-4899 (United States); Wang, X.-L., E-mail: xlwang@cityu.edu.hk [Department of Physics and Material Science, City University of Hong Kong 83 Tat Chee Ave., Kowloon (Hong Kong); City University of Hong Kong Shenzhen Research Institute, Shenzhen 518057 (China)

2016-05-23

Time-resolved synchrotron measurements were carried out to capture the structure evolution of an electrostatically levitated metallic-glass-forming liquid during free cooling. The experimental data shows a crossover in the liquid structure at ∼1000 K, about 115 K below the melting temperature and 150 K above the crystallization temperature. The structure change is characterized by a dramatic growth in the extended-range order below the crossover temperature. Molecular dynamics simulations have identified that the growth of the extended-range order was due to an increased correlation between solute atoms. These results provide structural evidence for a liquid-to-liquid-phase-transition in the supercooled metallic liquid.

Experimental study on liquid velocity in upward and downward two-phase flows

International Nuclear Information System (INIS)

Sun, X.; Paranjape, S.; Kim, S.; Ozar, B.; Ishii, M.

2003-01-01

Local characteristics of the liquid phase in upward and downward air-water two-phase flows were experimentally investigated in a 50.8-mm inner-diameter round pipe. An integral Laser Doppler Anemometry (LDA) system was used to measure the axial liquid velocity and its fluctuations. No effect of the flow direction on the liquid velocity radial profile was observed in single-phase liquid benchmark experiments. Local multi-sensor conductivity probes were used to measure the radial profiles of the bubble velocity and the void fraction. The measurement results in the upward and downward two-phase flows are compared and discussed. The results in the downward flow demonstrated that the presence of the bubbles tended to flatten the liquid velocity radial profile, and the maximum liquid velocity could occur off the pipe centerline, in particular at relatively low flow rates. However, the maximum liquid velocity always occurred at the pipe center in the upward flow. Also, noticeable turbulence enhancement due to the bubbles in the two-phase flows was observed in the current experimental flow conditions. Furthermore, the distribution parameter and the void weighted area-averaged drift velocity were obtained based on the definitions

A new method to describe two-phase solvent extraction based on net transport potential derived as linear combinations of forward and reverse constituents

International Nuclear Information System (INIS)

Nabeshima, Masahiro

1998-01-01

With the view to avoiding the difficulties encountered in estimating thermodynamic activities of the multiple chemical species in two-phase liquid system, a set of forward, reverse, net and total transport potentials are defined to represent the chemical state of a transferring solute during transient using bulk concentrations. The net transport potential corresponds to that in the conventional two-film model of diffusion-controlled processes. The overall driving forces of mass transport are redefined as the derivatives of the relevant transport potentials differentiated with respect to a state variable newly defined in terms of the bulk concentrations of the solute contained in both phases. Net and total quantities, i.e. transport potentials, overall driving forces and the molar fluxes are obtained as linear combinations of those for forward and reverse directions. The topical features presented by these quantities and their mutual relations are discussed in detail. The experimental new overall transport coefficient for U(VI) varied in accord with the changes in the theoretical net transport potential and overall driving force. The present method permits describing the extractive mass transport consistently both to forward and reverse directions of transport. (author)

Nuclide separation modeling through reverse osmosis membranes in radioactive liquid waste

OpenAIRE

Lee, Byung-Sik

2015-01-01

The aim of this work is to investigate the transport mechanism of radioactive nuclides through the reverse osmosis (RO) membrane and to estimate its effectiveness for nuclide separation from radioactive liquid waste. An analytical model is developed to simulate the RO separation, and a series of experiments are set up to confirm its estimated separation behavior. The model is based on the extended Nernst–Plank equation, which handles the convective flux, diffusive flux, and electromigration f...

Analysis of L-citrulline and L-arginine in Ficus deltoidea leaf extracts by reverse phase high performance liquid chromatography

Science.gov (United States)

Shafaei, Armaghan; Aisha, Abdalrahim F. A.; Siddiqui, Mohammad Jamshed Ahmad; Ismail, Zhari

2015-01-01

Background: Ficus deltoidea (FD) is one of the native plants widely distributed in several countries in Southeast Asia. Previous studies have shown that FD leaf possess antinociceptive, wound healing and antioxidant properties. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids and flavonoids. Objective: The aim was to develop a reverse phase high-performance liquid chromatography method with ultraviolet detection that involves precolumn derivatisation with O-phthaladehyde for simultaneous analysis of two amino acids L-citrulline and L-arginine in FD leaf extracts. Materials and Methods: An isocratic elution program consisting of methanol: acetonitrile: Water at 45:45:10 v/v (solvent A) and 0.1 M phosphate buffer pH 7.5 (solvent B) at A: B v/v ratio of 80:20 on Zorbax Eclipse C18 SB-Aq column (250 × 4.6 mm, 5 μm) were used. The flow rate was set at 1 ml/min and detection was carried out at 338 nm with 30 min separation time. Results: Good linearity for L-citrulline and L-arginine was obtained in the range 0.1-1000 μg/ml at R2 ≥ 0.998. The limit of detection and limit of quantification values for both L-citrulline and L-arginine were 1 and 5 μg/ml, respectively. The average of recoveries was in the range 94.94-101.95%, with relative standard deviation (%RSD) less than 3%. Intra- and inter-day precision was in the range 96.36-102.43% with RSD less than 2%. Conclusion: All validation parameters of the developed method indicate the method is reliable and efficient for simultaneous determination of L-citrulline and L-arginine for routine analysis of FD. PMID:25598632

Mapping of low molecular weight heparins using reversed phase ion pair liquid chromatography-mass spectrometry.

Science.gov (United States)

Li, Daoyuan; Chi, Lequan; Jin, Lan; Xu, Xiaohui; Du, Xuzhao; Ji, Shengli; Chi, Lianli

2014-01-01

Low molecular weight heparins (LMWHs) are structurally complex, highly sulfated and negatively charged, linear carbohydrate polymers prepared by chemical or enzymatic depolymerization of heparin. They are widely used as anticoagulant drugs possessing better bioavailability, longer half-life, and lower side effects than heparin. Comprehensive structure characterization of LMWHs is important for drug quality assurance, generic drug application, and new drug research and development. However, fully characterization of all oligosaccharide chains in LMWHs is not feasible for current available analytical technologies due to their structure complexity and heterogeneity. Fingerprinting profiling is an efficient way for LMWHs' characterization and comparison. In this work, we present a simple, sensitive, and powerful analytical approach for structural characterization of LMWHs. Two different LMWHs, enoxaparin and nadroparin, were analyzed using reversed phase ion pair electrospray ionization mass spectrometry (RPIP-ESI-MS). More than 200 components were identified, including major structures, minor structures, and process related impurities. This approach is robust for high resolution and complementary fingerprinting analysis of LMWHs. Copyright © 2013 Elsevier Ltd. All rights reserved.

Symmetry protected topological Luttinger liquids and the phase transition between them

Energy Technology Data Exchange (ETDEWEB)

None

2018-01-01

We show that a doped spin-1/2 ladder with antiferromagnetic intra-chain and ferromagnetic inter-chain coupling is a symmetry protected topologically non-trivial Luttinger liquid. Turning on a large easy-plane spin anisotropy drives the system to a topologically-trivial Luttinger liquid. Both phases have full spin gaps and exhibit power-law superconducting pair correlation. The Cooper pair symmetry is singlet $d_{xy}$ in the non-trivial phase and triplet $S_z=0$ in the trivial phase. The topologically non-trivial Luttinger liquid exhibits gapless spin excitations in the presence of a boundary, and it has no non-interacting or mean-field theory analog even when the fluctuating phase in the charge sector is pinned. As a function of the strength of spin anisotropy there is a topological phase transition upon which the spin gap closes. We speculate these Luttinger liquids are relevant to the superconductivity in metalized integer spin ladders or chains.

Visualization of velocity field and phase distribution in gas-liquid two-phase flow by NMR imaging

International Nuclear Information System (INIS)

Matsui, G.; Monji, H.; Obata, J.

2004-01-01

NMR imaging has been applied in the field of fluid mechanics, mainly single phase flow, to visualize the instantaneous flow velocity field. In the present study, NMR imaging was used to visualize simultaneously both the instantaneous phase structure and velocity field of gas-liquid two-phase flow. Two methods of NMR imaging were applied. One is useful to visualize both the one component of liquid velocity and the phase distribution. This method was applied to horizontal two-phase flow and a bubble rising in stagnant oil. It was successful in obtaining some pictures of velocity field and phase distribution on the cross section of the pipe. The other is used to visualize a two-dimensional velocity field. This method was applied to a bubble rising in a stagnant water. The velocity field was visualized after and before the passage of a bubble at the measuring cross section. Furthermore, the distribution of liquid velocity was obtained. (author)

Extraction Equilibrium of Acrylic Acid by Aqueous Two-Phase Systems Using Hydrophilic Ionic Liquids

International Nuclear Information System (INIS)

Lee, Yong Hwa; Lee, Woo Youn; Kim, Ki-Sub; Hong, Yeon Ki

2014-01-01

As an effective method for extraction of acrylic acid, aqueous two-phase systems based on morpholinium ionic liquids were used in this study. Effects of the alkyl chain length of cation in morpholinium ionic liquids on phase diagram and extraction efficiencies were investigated. Experimental results show that aqueous two phase systems can be formed by adding appropriate amount of morpholinium ionic liquids to aqueous K 2 HPO 4 solutions. It can be found that the ability of morpholinium ionic liquids for phase separation followed the order [HMMor][Br]>[OMMor][Br]>[BMMor][Br]>[EMMor][Br]. There was little difference between binodal curves of imidazolium ionic liquids and those of morpholinium ionic liquids. 50-90% of the extraction efficiency was observed for acrylic acid by aqueous two phase extraction of acrylic acid with morpholinium ionic liquids. It can be concluded that morpholinium ionic liquids/K 2 HPO 4 were effective for aqueous two phases extraction of acrylic acid comparing to imidazolium ionic liquids/K 2 HPO 4 systems because of their lower cost

Lyotropic Liquid Crystal Phases from Anisotropic Nanomaterials

Directory of Open Access Journals (Sweden)

Ingo Dierking

2017-10-01

Full Text Available Liquid crystals are an integral part of a mature display technology, also establishing themselves in other applications, such as spatial light modulators, telecommunication technology, photonics, or sensors, just to name a few of the non-display applications. In recent years, there has been an increasing trend to add various nanomaterials to liquid crystals, which is motivated by several aspects of materials development. (i addition of nanomaterials can change and thus tune the properties of the liquid crystal; (ii novel functionalities can be added to the liquid crystal; and (iii the self-organization of the liquid crystalline state can be exploited to template ordered structures or to transfer order onto dispersed nanomaterials. Much of the research effort has been concentrated on thermotropic systems, which change order as a function of temperature. Here we review the other side of the medal, the formation and properties of ordered, anisotropic fluid phases, liquid crystals, by addition of shape-anisotropic nanomaterials to isotropic liquids. Several classes of materials will be discussed, inorganic and mineral liquid crystals, viruses, nanotubes and nanorods, as well as graphene oxide.

Void fraction fluctuations in two-phase gas-liquid flow

International Nuclear Information System (INIS)

Ulbrich, R.

1987-01-01

Designs of the apparatus in which two-phase gas-liquid flow occurs are usually based on the mean value of parameters such as pressure drop and void fraction. The flow of two-phase mixtures generally presents a very complicated flow structure, both in terms of the unsteady formation on the interfacial area and in terms of the fluctuations of the velocity, pressure and other variables within the flow. When the gas void fraction is near 0 or 1 / bubble or dispersed flow regimes / then oscillations of void fraction are very small. The intermittent flow such as plug and slug/ froth is characterized by alternately flow portions of liquid and gas. It influences the change of void fractions in time. The results of experimental research of gas void fraction fluctuations in two-phase adiabatic gas-liquid flow in a vertical pipe are presented

Determination of Alkaloid Contents in Various Tissues of Coptis Chinensis Franch. by Reversed Phase-High Performance Liquid Chromatography and Ultraviolet Spectrophotometry.

Science.gov (United States)

Yang, Yanfang; Peng, Jingling; Li, Fangping; Liu, Xin; Deng, Meng; Wu, Hezhen

2017-05-01

A simple and intuitive method for optimizing the chemical constituents of Coptis Chinensis Franch. is important to assess its quality and clinical efficacy. An high performance liquid chromatography and ultraviolet spectrophotometry method was developed for the determination of berberine hydrochloride, palmatine chloride, jatrorrhizine hydrochloride, epiberberine, coptisine, columbamine and magnoflorine in various tissues (i.e., phloem, xylem and medulla) and rizhome of C. Chinensis Franch. The transection of rhizome from outside-in includes cork layer, cortex, phloem, cambium, xylem and medulla. Cork layer consists of dead cells, and therefore is not of any research significance. Cortex, phloem and cambium were almost impossible to separate, therefore they were studied as a whole in our experiments. They were collectively referred to as "phloem". The analytes were separated on a Gemini-NX C18 (250 mm × 4.6 mm, 5 μm) reversed phase column using a gradient elution of acetonitrile-0.03 mol/L ammonium acetate solution (containing 0.1% triethylamine and 0.6% ammonium hydroxide) as the mobile phase at a flow rate of 1.0 mL/min and UV detection at 270 nm. The method allowing the simultaneous quantification of seven major active constituents was optimized and validated for linearity, precision, accuracy, limits of detection (LOD) and quantification. The LOD ranged from 0.102 to 0.651 mg/mL (r ≥ 0.9993). Accuracy, precision and recovery were all within the required limits. The average recovery was between 100.14% and 102.75% and the relative standard deviations were spectrophotometry at 345 nm wavelength. Based on contents of the seven constituents and clustering result, this investigation suggests that there are significant differences in the distribution of seven alkaloids in the tissues examined. Furthermore, the total alkaloid content in xylem is relatively lower than that in phloem, medulla and rhizome. © The Author 2017. Published by Oxford University Press. All

First-principles study of the liquid and amorphous phases of In2Te3

Science.gov (United States)

Dragoni, D.; Gabardi, S.; Bernasconi, M.

2017-08-01

Structural, dynamical, and electronic properties of the liquid and amorphous phase of the In2Te3 compound have been studied by means of density functional molecular dynamics simulations. This system is of interest as a phase change material, undergoing a fast and reversible change between the crystalline and amorphous phases upon heating. It can be seen as a constituent of ternary InSbTe alloys which are receiving attention for application in electronic phase change memories. Amorphous models of In2Te3 300 -atom large have been generated by quenching from the melt by using different exchange and correlation functionals and different descriptions of the van der Waals interaction. It turns out the local bonding geometry of the amorphous phase is mostly tetrahedral with corner and edge sharing tetrahedra similar to those found in the crystalline phases of the InTe, In2Te3 , and In2Te5 compounds. Benchmark calculations on the crystalline α phase of In2Te3 in the defective zincblend geometry have also been performed. The calculations reveal that the high symmetric F 4 ¯3 m structure inferred experimentally from x-ray diffraction for the α phase must actually result from a random distribution of Te-Te bonds in different octahedral cages formed by the coalescence of vacancies in the In sublattice.

tRNA separation by high-performance liquid chromatography using an aggregate of ODS-Hypersil and trioctylmethylammonium chloride

NARCIS (Netherlands)

Bischoff, Rainer; Graeser, E.; Mclaughlin, L.W.

1983-01-01

High-performance liquid chromatography on a reversed-phase support treated with a tetraalkylammonium salt was used to separate tRNAs from baker's yeast. While resolution by this column appears to result from both anion-exchange and reversed-phase chromatography, it is the hydrophobic interactions

Liquid-gas phase transition and isospin fractionation in intermediate energy heavy ion collisions

International Nuclear Information System (INIS)

Xing Yongzhong; Liu Jianye; Guo Wenjun

2004-01-01

The liquid-gas phase transition in the heavy ion collisions and nuclear matter has been an important topic and got achievements, such as, based on the studies by H.Q. Song et al the critical temperature of liquid-gas phase transition enhances with increasing the mass of system and reduces as the increase of the neutron proton ratio of system. As authors know that both the liquid-gas phase transition and the isospin fractionation occur in the spinodal instability region at the nuclear density below the normal nuclear density. In particular, these two dynamical processes lead to the separation of nuclear matter into the liquid phase and gas phase. In this case to compare their dynamical behaviors is interested. The authors investigate the dependence of isospin fractionation degree on the mass and neutron proton ratio of system by using the isospin dependent quantum molecular dynamics model. The authors found that the degree of isospin fractionation (N/Z) n /(N/Z) imf decreases with increasing the mass of the system. This is just similar to the enhance of the critical temperature of liquid-gas phase transition T c as the increase of system mass. Because the enhance of T c is not favorable for the liquid-gas transition taking place, which reduces the isospin fractionation process and leads to decrease of (N/Z) n /(N/Z) imf . However the degree of isospin fractionation enhances with increasing the neutron proton ratio of the system. It is just corresponding to the reduce of T c of the liquid-gas phase transition as the increase of the isospin fractionation of the system. Because the reduce of T c enhances the liquid-gas phase transition process and also prompts the isospin fractionation process leading the increase of the isospin fractionation degree. To sum up, there are very similar dynamical behaviors for the degree of isospin fractionation and the critical temperature of the liquid-gas phase transition. So dynamical properties of the liquid-gas phase transition can

The shape of the melting curve and phase transitions in the liquid state

International Nuclear Information System (INIS)

Yahel, Eyal

2014-01-01

The phase diagram of elemental liquids has been found to be surprisingly rich, including variations in the melting curve and transitions in the liquid phase. The effect of these transitions on the shape of the melting curve is reviewed and analyzed. First-order phase transitions intersecting the melting curve imply piecewise continuous melting curves, with solid-solid transitions generating upward kinks or minima and liquid-liquid transitions generating downward kinks or maxima

Unconventional phase transitions in liquid crystals

Science.gov (United States)

Kats, E. I.

2017-12-01

According to classical textbooks on thermodynamics or statistical physics, there are only two types of phase transitions: continuous, or second-order, in which the latent heat L is zero, and first-order, in which L ≠ 0. Present-day textbooks and monographs also mention another, stand-alone type—the Berezinskii-Kosterlitz-Thouless transition, which exists only in two dimensions and shares some features with first- and second-order phase transitions. We discuss examples of non-conventional thermodynamic behavior (i.e., which is inconsistent with the theoretical phase transition paradigm now universally accepted). For phase transitions in smectic liquid crystals, mechanisms for nonconventional behavior are proposed and the predictions they imply are examined.

Liquid-phase and solid-phase radioimmunoassay with herpes simplex virus type 1 nucleocapsids

International Nuclear Information System (INIS)

Bystricka, M.; Rajcani, J.; Libikova, H.; Sabo, A.; Foeldes, O.; Sadlon, J.

1985-01-01

Liquid-phase radioimmunoassay and solid-phase radioimmunoassay are described using 125 I-labelled or immobilized nucleocapsids (NC) of herpes simplex virus (HSV) type1. These techniques appeared sensitive and specific for quantitation of HSV-NC antigens and corresponding antibodies. (author)

High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids.

Science.gov (United States)

Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

2008-07-11

Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method developed was successfully applied for primary screening of RTILs (>20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media.

Observation of diffusion phenomena of liquid phase with multiple components

International Nuclear Information System (INIS)

Eguchi, Wataru

1979-01-01

The diffusion phenomena of liquid phase with multiple components was directly observed, and the factors contributing to complex material transfer were investigated, comparing to the former experimental results. The most excellent method of observing the diffusion behavior of liquid phase used heretofore is to trace the time history of concentration distribution for each component in unsteady diffusion process. The method of directly observing the concentration distribution is usually classified into the analysis of diffused samples, the checking of radioactive isotope tracers, and the measurement of light refraction and transmission. The most suitable method among these is to trace this time history by utilizing the spectrophotometer of position scanning type. An improved spectrophotometer was manufactured for trial. The outline of the measuring system and the detail of the optical system of this new type spectrophotometer are explained. The resolving power for position measurement is described with the numerical calculation. As for the observation examples of the diffusion phenomena of liquid phase with multiple components, the diffusion of multiple electrolytes in aqueous solution, the observation of the material transfer phenomena accompanied by heterogeneous and single phase chemical reaction, and the observation of concentration distribution in the liquid diaphragm in a reaction absorption system are described. For each experimental item, the test apparatus, the sample material, the test process, the test results and the evaluation are explained in detail, and the diffusion phenomena of liquid phase with multiple components were pretty well elucidated. (Nakai, Y.)

Phase-field model of vapor-liquid-solid nanowire growth

Science.gov (United States)

Wang, Nan; Upmanyu, Moneesh; Karma, Alain

2018-03-01

We present a multiphase-field model to describe quantitatively nanowire growth by the vapor-liquid-solid (VLS) process. The free-energy functional of this model depends on three nonconserved order parameters that distinguish the vapor, liquid, and solid phases and describe the energetic properties of various interfaces, including arbitrary forms of anisotropic γ plots for the solid-vapor and solid-liquid interfaces. The evolution equations for those order parameters describe basic kinetic processes including the rapid (quasi-instantaneous) equilibration of the liquid catalyst to a droplet shape with constant mean curvature, the slow incorporation of growth atoms at the droplet surface, and crystallization within the droplet. The standard constraint that the sum of the phase fields equals unity and the conservation of the number of catalyst atoms, which relates the catalyst volume to the concentration of growth atoms inside the droplet, are handled via separate Lagrange multipliers. An analysis of the model is presented that rigorously maps the phase-field equations to a desired set of sharp-interface equations for the evolution of the phase boundaries under the constraint of force balance at three-phase junctions (triple points) given by the Young-Herring relation that includes torque term related to the anisotropy of the solid-liquid and solid-vapor interface excess free energies. Numerical examples of growth in two dimensions are presented for the simplest case of vanishing crystalline anisotropy and the more realistic case of a solid-liquid γ plot with cusped minima corresponding to two sets of (10 ) and (11 ) facets. The simulations reproduce many of the salient features of nanowire growth observed experimentally, including growth normal to the substrate with tapering of the side walls, transitions between different growth orientations, and crawling growth along the substrate. They also reproduce different observed relationships between the nanowire growth

Effect of silica nanoparticles on the phase inversion of liquid-liquid dispersions

International Nuclear Information System (INIS)

Asadabadi, Maliheh Raji; Abolghasemi, Hossein; Nasab, Payman Davoodi; Maragheh, Mohammad Ghannadi

2013-01-01

The effect of silica nanoparticles on phase inversion of liquid-liquid dispersions in a stirred vessel was investigated. The studied systems were toluene dispersed in water and vice versa. In the first set of experiments, phase inversion behavior of systems without Silica nanoparticles was evaluated and subsequent experiments were conducted in the presence of the nanoparticles. For this purpose, Silica nanoparticles of different concentrations (0.01, 0.03, 0.05, 0.07 wt%) were dispersed in water. The nanofluid stability was examined using an ultraviolet-visible (UV-vis) spectrophotometer. The results indicated that increase in silica nanoparticle concentrations up to 0.07 wt% led to increase in agitation speed of phase inversion 43-53.5% and 38.5-45% in the case of O/W and W/O dispersions, respectively. Consequently, the tendency of dispersions to inversion diminished as nanoparticle concentrations increased. Finally, 0.05 wt% of silica nanoparticle was selected as the optimum on the range studied

Flooding and flow reversal of two-phase annular flow

International Nuclear Information System (INIS)

Asahi, Y.

1978-01-01

The flooding and flow reversal conditions of two-phase annular flow are mathematically defined in terms of a characteristic function representing a force balance. Sufficiently below the flooding point in counter-current flow, the interface is smooth and the characteristic equation reduces to the Nusselt relationship. Just below flooding point and above the flow reversal point in cocurrent flow, the interface is 'wavy', so that the interfacial shear effect plays an important role. The theoretical analysis is compared with experimental results by others. It is suggested that the various length effects which have been experimentally observed may be accounted for by the spatial variation of the droplet entrainment. (Auth.)

Ginzburg-Landau equation and vortex liquid phase of Fermi liquid superconductors

International Nuclear Information System (INIS)

Ng, T-K; Tse, W-T

2007-01-01

In this paper we study the Ginzburg-Landau (GL) equation for Fermi liquid superconductors with strong Landau interactions F 0s and F 1s . We show that Landau interactions renormalize two parameters entering the GL equation, leading to the renormalization of the compressibility and superfluid density. The renormalization of the superfluid density in turn leads to an unconventional (2D) Berezinskii-Kosterlitz-Thouless (BKT) transition and vortex liquid phase. Application of the GL equation to describe underdoped high-T c cuprates is discussed

Profile of MIBI liquid phase radiopharmaceutical for myocardial imaging

International Nuclear Information System (INIS)

I Daruwati; ME Sriyani; NK Oekar; N Zainuddin; KA Hanafiah

2016-01-01

The 99m Tc-MIBI radiopharmaceutical has been used in nuclear medicine in Indonesia for myocardial imaging. BATAN researchers have mastered the technology to manufacture MIBI as a lyophilized kit. A reformulation of MIBI radiopharmaceutical has been conducted to improve the stability of the kit especially in the liquid-phase kit. Basically, radiopharmaceuticals in liquid form are not different from the dry kit. However in the manufacturing of liquid-phase kit, lyophilization process was not done. To improve the stability of liquid kit, a reformulation of the components was conducted by using two separate vials (Formulation 2) and the characteristics were compared with the one-vial formulation (Formulation 1). The MIBI Formulation 2 consists of two vials, vial A containing 0.06 mg of SnCl 2 2H 2 O and 2.6 mg Sodium Citrate 2H 2 O and vial B containing 0.5 mg of [Cu(MIBI) 4 ]BF 4 , 1 mg of cysteine hydrochloride, and 20 mg of mannitol. The purposes of this study were to determine the stability of two different formulations of MIBI as a liquid-phase kit, to compare their stability in different storage condition such as in refrigerator and freezer, and to compare the ratio of activities attained between target and nontarget organs after injection to animal model. As a diagnostic agent, MIBI was reconstituted with Technetium-99m as radionuclide tracer to 99m Tc-MIBI labeled compound. The radiochemical purity of 99m Tc-MIBI was determined by chromatography method using alumina thin-layer chromatography paper as the stationary phase and ethanol 95% as the mobile phase. The results showed MIBI Formulation 2 has a higher stability than Formulation 1. Formulation 2 also maintained a 96.68% radiochemical purity under 52-day storage and attained a target-to-nontarget activity ratio of 8.22. (author)

A novel evaluation method for extrapolated retention factor in determination of n-octanol/water partition coefficient of halogenated organic pollutants by reversed-phase high performance liquid chromatography.

Science.gov (United States)

Han, Shu-ying; Liang, Chao; Qiao, Jun-qin; Lian, Hong-zhen; Ge, Xin; Chen, Hong-yuan

2012-02-03

The retention factor corresponding to pure water in reversed-phase high performance liquid chromatography (RP-HPLC), k(w), was commonly obtained by extrapolation of retention factor (k) in a mixture of organic modifier and water as mobile phase in tedious experiments. In this paper, a relationship between logk(w) and logk for directly determining k(w) has been proposed for the first time. With a satisfactory validation, the approach was confirmed to enable easy and accurate evaluation of k(w) for compounds in question with similar structure to model compounds. Eight PCB congeners with different degree of chlorination were selected as a training set for modeling the logk(w)-logk correlation on both silica-based C(8) and C(18) stationary phases to evaluate logk(w) of sample compounds including seven PCB, six PBB and eight PBDE congeners. These eight model PCBs were subsequently combined with seven structure-similar benzene derivatives possessing reliable experimental K(ow) values as a whole training set for logK(ow)-logk(w) regressions on the two stationary phases. Consequently, the evaluated logk(w) values of sample compounds were used to determine their logK(ow) by the derived logK(ow)-logk(w) models. The logK(ow) values obtained by these evaluated logk(w) were well comparable with those obtained by experimental-extrapolated logk(w), demonstrating that the proposed method for logk(w) evaluation in this present study could be an effective means in lipophilicity study of environmental contaminants with numerous congeners. As a result, logK(ow) data of many PCBs, PBBs and PBDEs could be offered. These contaminants are considered to widely exist in the environment, but there have been no reliable experimental K(ow) data available yet. Copyright © 2011 Elsevier B.V. All rights reserved.

Void fraction prediction in two-phase flows independent of the liquid phase density changes

International Nuclear Information System (INIS)

Nazemi, E.; Feghhi, S.A.H.; Roshani, G.H.

2014-01-01

Gamma-ray densitometry is a frequently used non-invasive method to determine void fraction in two-phase gas liquid pipe flows. Performance of flow meters using gamma-ray attenuation depends strongly on the fluid properties. Variations of the fluid properties such as density in situations where temperature and pressure fluctuate would cause significant errors in determination of the void fraction in two-phase flows. A conventional solution overcoming such an obstacle is periodical recalibration which is a difficult task. This paper presents a method based on dual modality densitometry using Artificial Neural Network (ANN), which offers the advantage of measuring the void fraction independent of the liquid phase changes. An experimental setup was implemented to generate the required input data for training the network. ANNs were trained on the registered counts of the transmission and scattering detectors in different liquid phase densities and void fractions. Void fractions were predicted by ANNs with mean relative error of less than 0.45% in density variations range of 0.735 up to 0.98 gcm −3 . Applying this method would improve the performance of two-phase flow meters and eliminates the necessity of periodical recalibration. - Highlights: • Void fraction was predicted independent of density changes. • Recorded counts of detectors/void fraction were used as inputs/output of ANN. • ANN eliminated necessity of recalibration in changeable density of two-phase flows

Phase separation and structure formation in gadolinium based liquid and glassy metallic alloys

International Nuclear Information System (INIS)

Han, Junhee

2014-01-01

In this PhD research the liquid-liquid phase separation phenomena in Gd-based alloys was investigated in terms of phase equilibria, microstructure formation upon quenching the melt and corresponding magnetic properties of phase-separated metallic glasses. The phase diagrams of the binary subsystems Gd-Zr and Gd-Ti were experimentally reassessed. Especially the phase equilibria with the liquid phase could be determined directly by combining in situ high energy synchrotron X-ray diffraction with electrostatic levitation of the melt. The Gd-Zr system is of eutectic type with a metastable miscibility gap. The eutectic composition at 18 ± 2 at.% Zr, the liquidus line and the coexistence of bcc-Zr and bcc-Gd at elevated temperature could be determined. The Gd-Ti system is a monotectic system. The experimental observations in this work led to improved new Gd-Zr and Gd-Ti phase diagrams. The phase equilibria of the ternary Gd-Ti-Co system were analyzed for two alloy compositions. The XRD patterns for molten Gd 35 Ti 35 Co 30 gave direct evidence for the coexistence of two liquid phases formed by liquid-liquid phase separation. The first experimental and thermodynamic assessment of the ternary Gd-Ti-Co system revealed that the stable miscibility gap of binary Gd-Ti extends into the ternary Gd-Ti-Co system (up to about 30 at.% Co). New phase-separated metallic glasses were synthesized in Gd-TM-Co-Al (TM = Hf, Ti or Zr) alloys. The microstructure was characterized in terms of composition and cooling rate dependence of phase separation. Due to large positive enthalpy of mixing between Gd on the one side and Hf, Ti or Zr on the other side, the alloys undergo liquid-liquid phase separation during rapid quenching the melt. The parameters determining the microstructure development during phase separation are the thermodynamic properties of the liquid phase, kinetic parameters and quenching conditions. By controlling these parameters and conditions the microstructure can be

Isolation and quantitation of metallothionein isoforms using reversed-phase high-performance liquid chromatography

International Nuclear Information System (INIS)

Richards, M.P.; Darcey, S.E.; Steele, N.C.

1986-01-01

Reversed-phase HPLC (RP-HPLC) was used to isolate and quantify metallothionein (MT) isoforms from a variety of animal species and tissues. Separations were performed on C 18 radially compressed cartridge columns, eluted with a 2-step linear gradient of acetonitrile in 10 mM sodium phosphate, pH 7.0. Isoforms were detected by UV absorbance (214 nm) and by on-line interfacing with an atomic absorption spectrophotometer (HPLC-AA) to determine bound Zn, Cd and Cu. Rabbit liver and horse kidney MT's exhibited 7 distinct peaks on RP-HPLC, 2 of which were predominant (MT1 and 2). Pig liver and kidney MT2 yielded 2 subspecies on RP-HPLC, while MT1 yielded a single peak. Avian liver MT was unique from mammalian MT's in that MT2 was about tenfold more abundant than MT1. RP-HPLC and HPLC-AA were used to isolate and quantitate MT isoforms and their Zn content directly from cytosol. Quantitation was achieved by peak area integration and extrapolation from a standard curve of purified avian liver MT2. Both RP-HPLC and HPLC-AA had a lower detection limit of 1 + g of peptide and .1 μg of Zn. Recoveries (92-98%) were determined with labeled ( 35 S) MT and MT of known Zn content. Cytoplasmic MT-Zn in avian embryo hepatocytes cultured with added Zn was quantitated using HPLC-AA. In conclusion, both RP-HPLC and HPLC-AA are rapid and powerful separation techniques for the isolation, quantitation and characterization of the isoproteins comprising the MT gene family

Gas-liquid phase coexistence in a tetrahedral patchy particle model

International Nuclear Information System (INIS)

Romano, Flavio; Tartaglia, Piero; Sciortino, Francesco

2007-01-01

We evaluate the location of the gas-liquid coexistence line and of the associated critical point for the primitive model for water (PMW), introduced by Kolafa and Nezbeda (1987 Mol. Phys. 61 161). Besides being a simple model for a molecular network forming liquid, the PMW is representative of patchy proteins and novel colloidal particles interacting with localized directional short-range attractions. We show that the gas-liquid phase separation is metastable, i.e. it takes place in the region of the phase diagram where the crystal phase is thermodynamically favoured, as in the case of particles interacting via short-range attractive spherical potentials. We do not observe crystallization close to the critical point. The region of gas-liquid instability of this patchy model is significantly reduced as compared to that from equivalent models of spherically interacting particles, confirming the possibility of observing kinetic arrest in a homogeneous sample driven by bonding as opposed to packing. (fast track communication)

Plasma-liquid system with reverse vortex flow of 'tornado' type (TORNADO-LE)

International Nuclear Information System (INIS)

Nedybalyuk, O.A.; Chernyak, V.Ya.; Olszewski, S.V.

2010-01-01

The results of experimental investigations of the plasma in plasma-liquid system with reverse vortex flow of 'tornado' type are presented. Volt-ampere characteristic of discharge in the current range from 200 to 400 mA were measured. Emission spectra of plasma in range from 200 to 1100 nm were measured. Excitation temperatures (electronic T e * , vibrational T v * and rotational T r * ) were obtained. Emission spectra of hydroxyl OH were calculated.

LIQUID CHROMATOGRAPHIC / MASS SPECTROMETRIC DETERMINATION OF MORPHINE, CODEINE AND COCAINE IN HUMAN SERA USING A NEW INTERNAL SURFACE REVERSED PHASE COLUMN

OpenAIRE

Hattori, Hideki; Arinobu, Tetsuya; Iwai, Masae; Suzuki, Osamu; Seno, Hiroshi

2003-01-01

A new internal surface reversed phase column (Shim-pack MAYI-ODS) was used for analysis of morphine, codeine and cocaine in human sera by LC/MS/MS. The column enabled direct injection of crude biological samples without pretreatment realizing a rapid analytical procedure. Therecoveries of morphine, codeine and cocaine spiked into human sera were 50-60 %. The regression equations for morphine, codeine and cocaine in sera, using atropine as internal standard, showed good linearity in the ranges...

Origins of phase contrast in the atomic force microscope in liquids.

Science.gov (United States)

Melcher, John; Carrasco, Carolina; Xu, Xin; Carrascosa, José L; Gómez-Herrero, Julio; José de Pablo, Pedro; Raman, Arvind

2009-08-18

We study the physical origins of phase contrast in dynamic atomic force microscopy (dAFM) in liquids where low-stiffness microcantilever probes are often used for nanoscale imaging of soft biological samples with gentle forces. Under these conditions, we show that the phase contrast derives primarily from a unique energy flow channel that opens up in liquids due to the momentary excitation of higher eigenmodes. Contrary to the common assumption, phase-contrast images in liquids using soft microcantilevers are often maps of short-range conservative interactions, such as local elastic response, rather than tip-sample dissipation. The theory is used to demonstrate variations in local elasticity of purple membrane and bacteriophage 29 virions in buffer solutions using the phase-contrast images.

High-pressure phase diagrams of liquid CO2 and N2

Science.gov (United States)

Boates, Brian; Bonev, Stanimir

2011-06-01

The phase diagrams of liquid CO2 and N2 have been investigated using first-principles theory. Both materials exhibit transitions to conducting liquids at high temperatures (T) and relatively modest pressures (P). Furthermore, both liquids undergo polymerization phase transitions at pressures comparable to their solid counterparts. The liquid phase diagrams have been divided into several regimes through a detailed analysis of changes in bonding, as well as structural and electronic properties for pressures and temperatures up to 200 GPa and 10 000 K, respectively. Similarities and differences between the high- P and T behavior of these fluids will be discussed. Calculations of the Hugoniot are in excellent agreement with available experimental data. Work supported by NSERC, LLNL, and the Killam Trusts. Prepared by LLNL under Contract DE-AC52-07NA27344.

Behaviour of liquid films and flooding in counter-current two-phase flow, (1)

International Nuclear Information System (INIS)

Suzuki, Shin-ichi; Ueda, Tatsuhiro.

1978-01-01

This paper reports on the results of study of the behavior of liquid film and flooding in counter-current two phase flow, and the flow speed of gas phase was measured over the wide ranges of tube diameter, tube length, amount of liquid flow, viscosity and surface tension. Liquid samples used for this experiment were water, glycerol, and second octyl alcohol. The phenomena were observed with a high speed camera. The maximum thickness of liquid film was measured, and the effects of various factors on the flooding were investigated. The results of investigation were as follows. The big waves which cause the flooding were developed by the interaction of one of the waves on liquid film surface with gas phase flow. The flow speed of gas phase at the time of beginning of flooding increases with the reduction of amount of liquid flow and the increase of tube diameter. The flooding flow speed is reduced with the increase of tube length. The larger maximum film thickness at the time of no gas phase flow causes flooding at low gas phase flow speed. (Kato, T.)

Physico-Chemical Properties and Phase Behaviour of Pyrrolidinium-Based Ionic Liquids

Directory of Open Access Journals (Sweden)

Urszula Domańska

2010-04-01

Full Text Available A review of the relevant literature on 1-alkyl-1-methylpyrrolidinium-based ionic liquids has been presented. The phase diagrams for the binary systems of {1-ethyl-1-methylpyrrolidinium trifluoromethanesulfonate (triflate [EMPYR][CF3SO3] + water, or + 1-butanol} and for the binary systems of {1-propyl-1-methylpyrrolidinium trifluoromethanesulfonate (triflate [PMPYR][CF3SO3] + water, or + an alcohol (1-butanol, 1-hexanol, 1-octanol, 1-decanol} have been determined at atmospheric pressure using a dynamic method. The influence of alcohol chain length was discussed for the [PMPYR][CF3SO3]. A systematic decrease in the solubility was observed with an increase of the alkyl chain length of an alcohol. (Solid + liquid phase equilibria with complete miscibility in the liquid phase region were observed for the systems involving water and alcohols. The solubility of the ionic liquid increases as the alkyl chain length on the pyrrolidinium cation increases. The correlation of the experimental data has been carried out using the Wilson, UNIQUAC and the NRTL equations. The phase diagrams reported here have been compared to the systems published earlier with the 1-alkyl-1-methylpyrrolidinium-based ionic liquids. The influence of the cation and anion on the phase behaviour has been discussed. The basic thermal properties of pure ILs, i.e., melting temperature and the enthalpy of fusion, the solid-solid phase transition temperature and enthalpy have been measured using a differential scanning microcalorimetry technique.

Two-Order-Parameter Description of Liquids: Critical Phenomena and Phase Separation of Supercooled Liquids

OpenAIRE

Tanaka, Hajime

1997-01-01

Because of the isotropic and disordered nature of liquids, the anisotropy hidden in intermolecular interactions are often neglected. Accordingly, the order parameter describing a simple liquid has so far been believed to be only density. In contrast to this common sense, we propose that two order parameters, namely, density and bond order parameters, are required to describe the phase behavior of liquids since they intrinsically tend to form local bonds. This model gives us clear physical exp...

Effect of Foam on Liquid Phase Mobility in Porous Media

DEFF Research Database (Denmark)

Eftekhari, Ali Akbar; Farajzadeh, R.

2017-01-01

We investigate the validity of the assumption that foam in porous media reduces the mobility of gas phase only and does not impact the liquid-phase mobility. The foam is generated by simultaneous injection of nitrogen gas and a surfactant solution into sandstone cores and its strength is varied...... by changing surfactant type and concentration. We find, indeed, that the effect of foam on liquid-phase mobility is not pronounced and can be ignored. Our new experimental results and analyses resolve apparent discrepancies in the literature. Previously, some researchers erroneously applied relative...

Laser-induced separation of hydrogen isotopes in the liquid phase

International Nuclear Information System (INIS)

Beattie, W.; Freund, S.; Holland, R.; Maier, W.

1980-01-01

A process for separating hydrogen isotopes which comprises (A) forming a liquid phase of hydrogen-bearing feedstock compound at a temperature at which the spectral features of the feedstock compound are narrow enough or the absorption edges sharp enough to permit spectral features corresponding to the different hydrogen isotopes to be separated to be distinguished, (B) irradiating the liquid phase at said temperature with monochromatic radiation of a first wavelength which selectively or at least preferentially excites those molecules of said feedstock compound containing a first hydrogen isotope, and (C) subjecting the excited molecules to physical or chemical processes or a combination thereof whereby said first hydrogen isotope contained in said excited molecules is separated from other hydrogen isotopes contained in the unexcited molecules in said liquid phase

Auditory sensitivity to spectral modulation phase reversal as a function of modulation depth.

Science.gov (United States)

Buss, Emily; Grose, John

2018-01-01

The present study evaluated auditory sensitivity to spectral modulation by determining the modulation depth required to detect modulation phase reversal. This approach may be preferable to spectral modulation detection with a spectrally flat standard, since listeners appear unable to perform the task based on the detection of temporal modulation. While phase reversal thresholds are often evaluated by holding modulation depth constant and adjusting modulation rate, holding rate constant and adjusting modulation depth supports rate-specific assessment of modulation processing. Stimuli were pink noise samples, filtered into seven octave-wide bands (0.125-8 kHz) and spectrally modulated in dB. Experiment 1 measured performance as a function of modulation depth to determine appropriate units for adaptive threshold estimation. Experiment 2 compared thresholds in dB for modulation detection with a flat standard and modulation phase reversal; results supported the idea that temporal cues were available at high rates for the former but not the latter. Experiment 3 evaluated spectral modulation phase reversal thresholds for modulation that was restricted to either one or two neighboring bands. Flanking bands of unmodulated noise had a larger detrimental effect on one-band than two-band targets. Thresholds for high-rate modulation improved with increasing carrier frequency up to 2 kHz, whereas low-rate modulation appeared more consistent across frequency, particularly in the two-band condition. Experiment 4 measured spectral weights for spectral modulation phase reversal detection and found higher weights for bands in the spectral center of the stimulus than for the lowest (0.125 kHz) or highest (8 kHz) band. Experiment 5 compared performance for highly practiced and relatively naïve listeners, and found weak evidence of a larger practice effect at high than low spectral modulation rates. These results provide preliminary data for a task that may provide a better estimate of

Calculation of liquid-liquid equilibrium of aqueous two-phase systems using a chemical-theory-based excess Gibbs energy model

Directory of Open Access Journals (Sweden)

Pessôa Filho P. A.

2004-01-01

Full Text Available Mixtures containing compounds that undergo hydrogen bonding show large deviations from ideal behavior. These deviations can be accounted for through chemical theory, according to which the formation of a hydrogen bond can be treated as a chemical reaction. This chemical equilibrium needs to be taken into account when applying stability criteria and carrying out phase equilibrium calculations. In this work, we illustrate the application of the stability criteria to establish the conditions under which a liquid-phase split may occur and the subsequent calculation of liquid-liquid equilibrium using a chemical-theory-modified Flory-Huggins equation to describe the non ideality of aqueous two-phase systems composed of poly(ethylene glycol and dextran. The model was found to be able to correlate ternary liquid-liquid diagrams reasonably well by simple adjustment of the polymer-polymer binary interaction parameter.

Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

Science.gov (United States)

Kahsay, Getu; Shraim, Fairouz; Villatte, Philippe; Rotger, Jacques; Cassus-Coussère, Céline; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

2013-03-05

A simple, robust and fast high-performance liquid chromatographic method is described for the analysis of oxytetracycline and its related impurities. The principal peak and impurities are all baseline separated in 20 min using an Inertsil C₈ (150 mm × 4.6 mm, 5 μm) column kept at 50 °C. The mobile phase consists of a gradient mixture of mobile phases A (0.05% trifluoroacetic acid in water) and B (acetonitrile-methanol-tetrahydrofuran, 80:15:5, v/v/v) pumped at a flow rate of 1.3 ml/min. UV detection was performed at 254 nm. The developed method was validated for its robustness, sensitivity, precision and linearity in the range from limit of quantification (LOQ) to 120%. The limits of detection (LOD) and LOQ were found to be 0.08 μg/ml and 0.32 μg/ml, respectively. This method allows the separation of oxytetracycline from all known and 5 unknown impurities, which is better than previously reported in the literature. Moreover, the simple mobile phase composition devoid of non-volatile buffers made the method suitable to interface with mass spectrometry for further characterization of unknown impurities. The developed method has been applied for determination of related substances in oxytetracycline bulk samples available from four manufacturers. The validation results demonstrate that the method is reliable for quantification of oxytetracycline and its impurities. Copyright © 2012 Elsevier B.V. All rights reserved.

Development of an analytical method for the determination of histamine in fish by liquid chromatography of high performance in reverse phase

International Nuclear Information System (INIS)

Valverde Chavarria, Juan Carlos; Barquero Quiros, Mirian

2004-01-01

The histamine is a biogenic amine able to promote allergic intoxications in sensitive persons. For this reason is necessary to have a method of analysis with sensitivity, precision and accuracy able to quantify lower amounts than actual FDA Normative sets. A reverse phase chromatographic method was developed. To identify and quantify histamine through automatic generation of histamine derivative of OPA, using an ultraviolet detector, performance parameters of developed method were adequate to quantification of histamine amount lower than FDA Normative. (Author) [es

Two-dimensional solid-phase extraction strategy for the selective enrichment of aminoglycosides in milk.

Science.gov (United States)

Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

2017-03-01

An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization and validation of a reversed-phase high performance liquid chromatography method for the measurement of bovine liver methylmalonyl-coenzyme a mutase activity.

Science.gov (United States)

Ouattara, Bazoumana; Duplessis, Mélissa; Girard, Christiane L

2013-10-16

Methylmalonyl-CoA mutase (MCM) is an adenosylcobalamin-dependent enzyme that catalyses the interconversion of (2R)-methylmalonyl-CoA to succinyl-CoA. In humans, a deficit in activity of MCM, due to an impairment of intracellular formation of adenosylcobalamin and methylcobalamin results in a wide spectrum of clinical manifestations ranging from moderate to fatal. Consequently, MCM is the subject of abundant literature. However, there is a lack of consensus on the reliable method to monitor its activity. This metabolic pathway is highly solicited in ruminants because it is essential for the utilization of propionate formed during ruminal fermentation. In lactating dairy cows, propionate is the major substrate for glucose formation. In present study, a reversed-phase high performance liquid chromatography (RP-HPLC) was optimized and validated to evaluate MCM activity in bovine liver. The major aim of the study was to describe the conditions to optimize reproducibility of the method and to determine stability of the enzyme and its product during storage and processing of samples. Specificity of the method was good, as there was no interfering peak from liver extract at the retention times corresponding to methylmalonyl-CoA or succinyl-CoA. Repeatability of the method was improved as compared to previous RP-HPLC published data. Using 66 μg of protein, intra-assay coefficient of variation (CV) of specific activities, ranged from 0.90 to 8.05% and the CV inter-day was 7.40%. Storage and processing conditions (frozen homogenate of fresh tissue vs. fresh homogenate of tissue snapped in liquid nitrogen) did not alter the enzyme activity. The analyte was also stable in liver crude extract for three frozen/thawed cycles when stored at -20°C and thawed to room temperature. The improved method provides a way for studying the effects of stages of lactation, diet composition, and physiology in cattle on MCM activity over long periods of time, such as a complete lactation period

Liquid Phase Sintering of Highly Alloyed Stainless Steel

DEFF Research Database (Denmark)

Mathiesen, Troels

1996-01-01

Liquid phase sintering of stainless steel is usually applied to improve corrosion resistance by obtaining a material without an open pore system. The dense structure normally also give a higher strength when compared to conventional sintered steel. Liquid phase sintrering based on addition...... of boride to AISI 316L type steels have previously been studied, but were found to be sensitive to intergranular corrosion due to formation of intermetallic phases rich in chromium and molybdenum. In order to improve this system further, new investigations have focused on the use of higher alloyed stainless...... steel as base material. The stainless base powders were added different amounts and types of boride and sintered in hydrogen at different temperatures and times in a laboratory furnace. During sintering the outlet gas was analyzed and subsequently related to the obtained microstructure. Thermodynamic...

A multi-phase equation of state for solid and liquid lead

International Nuclear Information System (INIS)

Robinson, C.M.

2004-01-01

This paper considers a multi-phase equation of state for solid and liquid lead. The thermodynamically consistent equation of state is constructed by calculating separate equations of state for the solid and liquid phases. The melt curve is the curve in the pressure, temperature plane where the Gibb's free energy of the solid and liquid phases are equal. In each phase a complete equation of state is obtained using the assumptions that the specific heat capacity is constant and that the Grueneisen parameter is proportional to the specific volume. The parameters for the equation of state are obtained from experimental data. In particular they are chosen to match melt curve and principal Hugoniot data. Predictions are made for the shock pressure required for melt to occur on shock and release

Kinetic and thermodynamic study of the transfer of anionic polyamidoamine dendrimers across two immiscible liquids

International Nuclear Information System (INIS)

Gonzalez-Fuentes, Miguel A.; Manriquez, J.; Antano-Lopez, R.; Godinez, Luis A.

2011-01-01

The kinetics and thermodynamics for the phase transfer of carboxyl-terminated polyamidoamine (PAMAM) dendrimers across the water/dichloroethane interface were analyzed by cyclic voltammetry and electrochemical impedance spectroscopy. A three phase junction was employed by inserting a cylindrical gold electrode through the liquid-liquid interface. The reversible redox species decamethylferrocene (DMFc) was used in the organic phase in order to promote dendrimer transfer. It was found that the electrochemical behaviour of DMFc at the gold/dichloroethane interface depends on the generation and concentration of the dendrimer species in the aqueous phase. In addition, it was observed that the electrochemically driven transfer of these macromolecules corresponds to a quasi-reversible process. The data obtained from thermodynamic studies indicate that dendrimers are transferred between the two phases under study by an entropy controlled process.

Measurement of Liquid-Metal Two-Phase Flow with a Dynamic Neutron Radiography

International Nuclear Information System (INIS)

Cha, J. E.; Lim, I. C.; Kim, H. R.; Kim, C. M.; Nam, H. Y.; Saito, Y.

2005-01-01

The dynamic neutron radiography(DNR) has complementary characteristics to X-ray radiography and is suitable to visualization and measurement of a multi-phase flow research in a metallic duct and liquid metal flow. The flow-field information of liquid metal system is very important for the safety analysis of fast breeder reactor and the design of the spallation target of accelerator driven system. A DNR technique was applied to visualize the flow field in the gas-liquid metal two-phase flow with the HANARO-beam facility. The lead bismuth eutectic and the nitrogen gas were used to construct the two-phase flow field in the natural circulation U-channel. The two-phase flow images in the riser were taken at various combinations of the liquid flow and gas flow with high frame-rate neutron radiography at 1000 fps

Liquid-liquid extraction in flow analysis: A critical review

Energy Technology Data Exchange (ETDEWEB)

Silvestre, Cristina I.C.; Santos, Joao L.M. [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Lima, Jose L.F.C., E-mail: limajlfc@ff.up.pt [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Zagatto, Elias A.G. [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, P.O. Box 96, Piracicaba 13400-970 (Brazil)

2009-10-12

Liquid-liquid extractions (LLE) are a common sample pre-treatment in many analytical applications. This review aims at providing a critical overview of the distinct automated continuous flow-based approaches that were developed for liquid-liquid extraction with the purpose of pre-concentration and/or separation of multiple analytes, such as ultra-trace metal and metalloid species, phenolic compounds, surfactants, pharmaceuticals, etc., hyphenated with many detection technique such as UV/vis spectrophotometry, atomic spectrometric detection systems and luminescent detectors, including distinct extraction strategies and applications like single and multiple extraction schemes, wetting film extraction, supported liquid membrane extraction, back extraction, closed-loop systems and the utilisation of zone sampling, chromatomembranes and iterative reversal techniques. The analytical performance of the developed flow-based LLE methods and the influence of flow manifold components such as the segmenter, extraction coil and phase separator, is emphasised and object of discussion. An overall presentation of each system components, selectivity, advantages and shortcomings is carried out and exemplified with selected applications.

Gas holdup in a reciprocating plate bioreactor: Non-Newtonian - liquid phase

Directory of Open Access Journals (Sweden)

Naseva Olivera S.

2002-01-01

Full Text Available The gas holdup was studied in non-newtonian liquids in a gas-liquid and gas-liquid-solid reciprocating plate bioreactor. Aqueous solutions of carboxy methyl cellulose (CMC; Lucel, Lučane, Yugoslavia of different degrees of polymerization (PP 200 and PP 1000 and concentration (0,5 and 1%, polypropylene spheres (diameter 8.3 mm; fraction of spheres: 3.8 and 6.6% by volume and air were used as the liquid, solid and gas phase. The gas holdup was found to be dependent on the vibration rate, the superficial gas velocity, volume fraction of solid particles and Theological properties of the liquid ohase. Both in the gas-liquid and gas-liquid-solid systems studied, the gas holdup increased with increasing vibration rate and gas flow rate. The gas holdup was higher in three-phase systems than in two-phase ones under otter operating conditions being the same. Generally the gas holdup increased with increasing the volume fraction of solid particles, due to the dispersion action of the solid particles, and decreased with increasing non-Newtonian behaviour (decreasing flow index i.e. with increasing degree of polymerization and solution concentration of CMC applied, as a result of gas bubble coalescence.

Variation in pH of Model Secondary Organic Aerosol during Liquid-Liquid Phase Separation.

Science.gov (United States)

Dallemagne, Magda A; Huang, Xiau Ya; Eddingsaas, Nathan C

2016-05-12

The majority of atmospheric aerosols consist of both organic and inorganic components. At intermediate relative humidity (RH), atmospheric aerosol can undergo liquid-liquid phase separation (LLPS) in which the organic and inorganic fractions segregate from each other. We have extended the study of LLPS to the effect that phase separation has on the pH of the overall aerosols and the pH of the individual phases. Using confocal microscopy and pH sensitive dyes, the pH of internally mixed model aerosols consisting of polyethylene glycol 400 and ammonium sulfate as well as the pH of the organic fraction during LLPS have been directly measured. During LLPS, the pH of the organic fraction was observed to increase to 4.2 ± 0.2 from 3.8 ± 0.1 under high RH when the aerosol was internally mixed. In addition, the high spatial resolution of the confocal microscope allowed us to characterize the composition of each of the phases, and we have observed that during LLPS the organic shell still contains large quantities of water and should be characterized as an aqueous organic-rich phase rather than simply an organic phase.

Improved method for the determination of the cortisol production rate using high-performance liquid chromatography and liquid scintillation counting

NARCIS (Netherlands)

van Ingen, H. E.; Endert, E.

1988-01-01

Two new methods for the determination of the cortisol production rate using reversed-phase high-performance liquid chromatography are described. One uses ultraviolet detection at 205 nm, the other on-line post-column derivatization with benzamidine, followed by fluorimetric detection. The specific

Pressure Dependence of the Liquid-Liquid Phase Transition of Nanopore Water Doped Slightly with Hydroxylamine, and a Phase Behavior Predicted for Pure Water

Science.gov (United States)

Nagoe, Atsushi; Iwaki, Shinji; Oguni, Masaharu; Tôzaki, Ken-ichi

2014-09-01

Phase transition behaviors of confined pure water and confined water doped with a small amount of hydroxylamine (HA) with a mole fraction of xHA = 0.03 were examined by high-pressure differential thermal analyses at 0.1, 50, 100, and 150 MPa; the average diameters of silica pores used were 2.0 and 2.5 nm. A liquid-liquid phase transition (LLPT) of the confined HA-doped water was clearly observed and its pressurization effect could be evaluated, unlike in the experiments on undoped water. It was found that pressurization causes the transition temperature (Ttrs) to linearly decrease, indicating that the low-temperature phase has a lower density than the high-temperature one. Transition enthalpy (ΔtrsH) decreased steeply with increasing pressure. Considering the linear decrease in Ttrs with increasing pressure, the steep decrease in ΔtrsH indicates that the LLPT effect of the HA-doped water attenuates with pressure. We present a new scenario of the phase behavior concerning the LLPT of pure water based on the analogy from the behavior of slightly HA-doped water, where a liquid-liquid critical point (LLCP) and a coexistence line are located in a negative-pressure regime but not in a positive-pressure one. It is reasonably understood that doping a small amount of HA into water results in negative chemical pressurization and causes the LLPT to occur even at ambient pressure.

Heat transfer by gas-liquid mixture in forced turbulent flow with weak vaporization of the liquid phase (1962); Transfert de chaleur par melange de liquide et de gaz en convection forcee turbulente avec faible vaporisation de la phase liquide (1962)

Energy Technology Data Exchange (ETDEWEB)

Huyghe, J; Mondin, G [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

1962-07-01

The present study deals with measures of heat transfer and pressure drop in two-phase liquid flow. The stream is of annular dispersed type, obtained by introducing a small quantity of liquid in a gas turbulent flow. The heat transfer experiments are performed without vaporization of the liquid phase. A notable improvement of the heat transfer coefficient of such a stream is observed, compared with a gas-alone or liquid-alone flow. The improvement concerning the gas-alone is of about 20 when it is compared with the same gas Reynolds's number, of about 8 when it is compared with the same total mass flow rate. A hydrodynamic study of the flow pattern lets us know the original structure of the flow, and allows to foresee the experimental results by means of a simplified theory. (authors) [French] II est fait etat de mesures de transfert thermique et de perte de charge dans un ecoulement en double phase gaz-liquide. L'ecoulement est du type annulaire disperse, obtenu par injection d'une faible quantite de liquide dans un ecoulement gazeux en regime turbulent. Les experiences de transfert thermique sont menees sans vaporisation de la phase liquide. On note une amelioration sensible du coefficient de transfert thermique dans un tel ecoulement par rapport a un ecoulement de gaz seul ou de liquide seul. L'augmentation est de l'ordre de 20 par rapport au gaz seul si on opere a meme nombre de REYNOLDS du gaz, de l'ordre de 8 si on opere a meme debit massique total. Une etude hydrodynamique rapide de l'ecoulement permet de connaitre la structure originale de l'ecoulement, puis de prevoir par une theorie simplifiee le phenomene thermique observe. (auteurs)

Problems of selectivity in liquid-phase oxidation

Energy Technology Data Exchange (ETDEWEB)

Emanuel, N M

1978-07-01

Based on a kinetic analysis of a generalized scheme for radical-chain process and on published experimental results, factors determining the selectivities of various liquid-phase oxidations of organic compounds are examined, including the kinetic chain length, molecular and chain decomposition of products, and competing routes in the initiated oxidation or autoxidation of hydrocarbons to peroxides. Also discussed are selective inhibition of undesirable routes in chain reactions, e.g., styrene and acetaldehyde co-oxidation; activation of molecular oxygen by variable-valence metal compounds used as homogeneous catalysts; modeling of fermentative processes by oxidation of hydrocarbons in complex catalytic systems, e.g., hydroxylation of alkanes, epoxidation or carbonylation of olefins, or oxidation of alcohols and ketones to acids; and the mechanisms of heterogeneous catalysis in liquid-phase reactions, e.g., oxidation of alkylaromatic hydrocarbons to peroxides and co-oxidation of propylene and acetaldehyde.

Development and validation of reversed-phase high performance liquid chromatographic method for analysis of cephradine in human plasma samples

International Nuclear Information System (INIS)

Ahmad, M.; Usman, M.; Madni, A.; Akhtar, N.; Khalid, N.; Asghar, W.

2010-01-01

An HPLC method with high precision, accuracy and selectivity was developed and validated for the assessment of cephradine in human plasma samples. The extraction procedure was simple and accurate with single step followed by direct injection of sample into HPLC system. The extracted cephradine in spiked human plasma was separated and quantitated using reversed phase C/sub 18/ column and UV detection wavelength of 254 nm. The optimized mobile phase of new composition of 0.05 M potassium dihydrogen phosphate (pH 3.4)-acetonitrile (88: 12) was pumped at an optimum flow rate of 1 mL.min/sup 1/. The method resulted linearity in the concentration range 0.15- 20 micro g mL/sup -1/. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.150 Microg.mL/sup -1/, respectively. The accuracy of method was 98.68 %. This method can 1>e applied for bioequivalence studies and therapeutic drug monitoring as well as for the routine analysis of cephradine. (author)

Study of plasma equilibrium during the AC current reversal phase in STOR-M

International Nuclear Information System (INIS)

Xiao, C.

2002-01-01

Alternating current (AC) tokamak operation and equilibrium studies have been performed on the STOR-M tokamak. The recent experiments have achieved consistent smooth current reversal through the implementation of a hybrid digital-analog position controller and by careful density control. In order to study the plasma equilibrium during the current reversal phase with negligible rotational transform, a segmented limiter with four isolated conducting plates has been installed. The plates can be connected outside the vacuum vessel, which allows measurements of currents flowing between limiter plates. When the current reversal is smooth with zero dwell time, the hydrogen line emission level and electron density remain finite, indicating a finite particle confinement. The current from the top to the bottom limiter plate is also finite and its direction is consistent with that of the grad-B drift. The observation suggests that the limiter and other conducting structures surrounding the plasmas plays the role, during the current reversal phase of AC tokamak operation, to short out the charge separation arising from the grad-B drift and to maintain a finite particle confinement. (author)

Novel materials and methods for solid-phase extraction and liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

1997-06-24

This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

A Simple Approach to Characterize Gas-Aqueous Liquid Two-phase Flow Configuration Based on Discrete Solid-Liquid Contact Electrification.

Science.gov (United States)

Choi, Dongwhi; Lee, Donghyeon; Kim, Dong Sung

2015-10-14

In this study, we first suggest a simple approach to characterize configuration of gas-aqueous liquid two-phase flow based on discrete solid-liquid contact electrification, which is a newly defined concept as a sequential process of solid-liquid contact and successive detachment of the contact liquid from the solid surface. This approach exhibits several advantages such as simple operation, precise measurement, and cost-effectiveness. By using electric potential that is spontaneously generated by discrete solid-liquid contact electrification, the configurations of the gas-aqueous liquid two-phase flow such as size of a gas slug and flow rate are precisely characterized. According to the experimental and numerical analyses on parameters that affect electric potential, gas slugs have been verified to behave similarly to point electric charges when the measuring point of the electric potential is far enough from the gas slug. In addition, the configuration of the gas-aqueous liquid two-phase microfluidic system with multiple gas slugs is also characterized by using the presented approach. For a proof-of-concept demonstration of using the proposed approach in a self-triggered sensor, a gas slug detector with a counter system is developed to show its practicality and applicability.

Reverse bistable effect in ferroelectric liquid crystal devices with ultra-fast switching at low driving voltage.

Science.gov (United States)

Guo, Qi; Zhao, Xiaojin; Zhao, Huijie; Chigrinov, V G

2015-05-15

In this Letter, reverse bistable effect with deep-sub-millisecond switching time is first reported in ferroelectric liquid crystal (FLC) devices using a homogeneous photo-alignment technique. It is indicated by our experimental results that both the anchoring energy and the dielectric property of the FLC's alignment layer is critical for the existence of the reverse bistable effect. In addition, with the derived criteria of the reverse bistable effect, we quantitatively analyze the switching dynamics of the reverse bistable FLC and the transition condition between the traditional bistability and our presented reverse bistability. Moreover, the fabricated FLC device exhibits an ultra-fast switching of ∼160  μs and a high contrast ratio of 1000:1, both of which were measured at a low driving voltage of 11 V. The featured deep-sub-millisecond switching time is really advantageous for our presented reverse bistable FLC devices, which enables a significant quality improvement of the existing optical devices, as well as a wide range of new applications in photonics and display areas.

Glass and liquid phase diagram of a polyamorphic monatomic system

Science.gov (United States)

Reisman, Shaina; Giovambattista, Nicolas

2013-02-01

We perform out-of-equilibrium molecular dynamics (MD) simulations of a monatomic system with Fermi-Jagla (FJ) pair potential interactions. This model system exhibits polyamorphism both in the liquid and glass state. The two liquids, low-density (LDL) and high-density liquid (HDL), are accessible in equilibrium MD simulations and can form two glasses, low-density (LDA) and high-density amorphous (HDA) solid, upon isobaric cooling. The FJ model exhibits many of the anomalous properties observed in water and other polyamorphic liquids and thus, it is an excellent model system to explore qualitatively the thermodynamic properties of such substances. The liquid phase behavior of the FJ model system has been previously characterized. In this work, we focus on the glass behavior of the FJ system. Specifically, we perform systematic isothermal compression and decompression simulations of LDA and HDA at different temperatures and determine "phase diagrams" for the glass state; these phase diagrams varying with the compression/decompression rate used. We obtain the LDA-to-HDA and HDA-to-LDA transition pressure loci, PLDA-HDA(T) and PHDA-LDA(T), respectively. In addition, the compression-induced amorphization line, at which the low-pressure crystal (LPC) transforms to HDA, PLPC-HDA(T), is determined. As originally proposed by Poole et al. [Phys. Rev. E 48, 4605 (1993)], 10.1103/PhysRevE.48.4605 simulations suggest that the PLDA-HDA(T) and PHDA-LDA(T) loci are extensions of the LDL-to-HDL and HDL-to-LDL spinodal lines into the glass domain. Interestingly, our simulations indicate that the PLPC-HDA(T) locus is an extension, into the glass domain, of the LPC metastability limit relative to the liquid. We discuss the effects of compression/decompression rates on the behavior of the PLDA-HDA(T), PHDA-LDA(T), PLPC-HDA(T) loci. The competition between glass polyamorphism and crystallization is also addressed. At our "fast rate," crystallization can be partially suppressed and the

Nanoscale Phase Stability Reversal During the Nucleation and Growth of Titanium Oxide Minerals

Science.gov (United States)

Hummmer, D. R.; Heaney, P. J.; Kubicki, J. D.; Kent, P. R.; Post, J. E.

2008-12-01

Fine-grained titanium oxide minerals are important in soils, where they affect a variety of geochemical processes. They are also industrially important as catalysts, pigments, food additives, and dielectrics. Recent research has indicated an apparent reversal of thermodynamic stability between TiO2 phases at the nanoscale thought to be caused by an increased contribution of surface energy to the total free energy. Time-resolved X-ray diffraction (XRD) experiments in which titanium oxides crystallize from aqueous TiCl4 solutions confirm that anatase, a metastable phase, is always the first phase to nucleate under our range of initial conditions. Rutile peaks are observed only minutes after the first appearance of anatase, after which anatase abundance slowly decreases while rutile continues to form. Whole pattern refinement of diffraction data reveals that lattice constants of both phases increase throughout the crystallization process. In addition, transmission electron microscope (TEM) observations and kinetic modeling indicate that anatase does not undergo a solid-state transformation to the rutile structure as once thought. Instead, anatase appears to re-dissolve and then feed the growth of already nucleated rutile nanocrystals. Density functional theory (DFT) calculations were employed to model 1, 2, and 3 nm particles of both mineral phases. The total surface energies calculated from these models did yield lower values for anatase than for rutile by 8-13 kJ/mol depending on particle size, indicating that surface free energy is sufficient to account for stability reversal. However, these whole-particle surface energies were much higher than the sum of energies of each particle's constituent crystallographic surfaces. We attribute the excess energy to defects associated with the edges and corners of nanoparticles, which are not present on a 2-D periodic surface. This previously unreported edge and corner energy may play a dominant role in the stability reversal

Search for the first-order liquid-to-liquid phase transition in low-temperature confined water by neutron scattering

Science.gov (United States)

Chen, Sow-Hsin; Wang, Zhe; Kolesnikov, Alexander I.; Zhang, Yang; Liu, Kao-Hsiang

2013-02-01

It has been conjectured that a 1st order liquid-to-liquid (L-L) phase transition (LLPT) between high density liquid (HDL) and low density liquid (LDL) in supercooled water may exist, as a thermodynamic extension to the liquid phase of the 1st order transition established between the two bulk solid phases of amorphous ice, the high density amorphous ice (HDA) and the low density amorphous ice (LDA). In this paper, we first recall our previous attempts to establish the existence of the 1st order L-L phase transition through the use of two neutron scattering techniques: a constant Q elastic diffraction study of isobaric temperature scan of the D2O density, namely, the equation of state (EOS) measurements. A pronounced density hysteresis phenomenon in the temperature scan of the density above P = 1500 bar is observed which gives a plausible evidence of crossing the 1st order L-L phase transition line above this pressure; an incoherent quasi-elastic scattering measurements of temperature-dependence of the α-relaxation time of H2O at a series of pressures, namely, the study of the Fragile-to-Strong dynamic crossover (FSC) phenomenon as a function of pressure which we interpreted as the results of crossing the Widom line in the one-phase region. In this new experiment, we used incoherent inelastic neutron scattering (INS) to measure the density of states (DOS) of H atoms in H2O molecules in confined water as function of temperature and pressure, through which we may be able to follow the emergence of the LDL and HDL phases at supercooled temperature and high pressures. We here report for the first time the differences of librational and translational DOSs between the hypothetical HDL and LDL phases, which are similar to the corresponding differences between the well-established HDA and LDA ices. This is plausible evidence that the HDL and LDL phases are the thermodynamic extensions of the corresponding amorphous solid water HDA and LDA ices.

Electrically Tunable Reflective Terahertz Phase Shifter Based on Liquid Crystal

Science.gov (United States)

Yang, Jun; Xia, Tianyu; Jing, Shuaicheng; Deng, Guangsheng; Lu, Hongbo; Fang, Yong; Yin, Zhiping

2018-02-01

We present a reflective spatial phase shifter which operates at terahertz regime above 325 GHz. The controllable permittivity of the nematic liquid crystals was utilized to realize a tunable terahertz (THz) reflective phase shifter. The reflective characteristics of the terahertz electromagnetic waves and the liquid crystal parameters were calculated and analyzed. We provide the simulation results for the effect of the incident angle of the plane wave on the reflection. The experiment was carried out considering an array consisting of 30 × 30 patch elements, printed on a 20 × 20 mm quartz substrate with 1-mm thickness. The phase shifter provides a tunable phase range of 300° over the frequency range of 325 to 337.6 GHz. The maximum phase shift of 331° is achieved at 330 GHz. The proposed phase shifter is a potential candidate for THz applications, particularly for reconfigurable reflectarrays.

A liquid-liquid transition in supercooled aqueous solution related to the HDA-LDA transition

Science.gov (United States)

Woutersen, Sander; Ensing, Bernd; Hilbers, Michiel; Zhao, Zuofeng; Angell, C. Austen

2018-03-01

Simulations and theory suggest that the thermodynamic anomalies of water may be related to a phase transition between two supercooled liquid states, but so far this phase transition has not been observed experimentally because of preemptive ice crystallization. We used calorimetry, infrared spectroscopy, and molecular dynamics simulations to investigate a water-rich hydrazinium trifluoroacetate solution in which the local hydrogen bond structure surrounding a water molecule resembles that in neat water at elevated pressure, but which does not crystallize upon cooling. Instead, this solution underwent a sharp, reversible phase transition between two homogeneous liquid states. The hydrogen-bond structures of these two states are similar to those established for high- and low-density amorphous (HDA and LDA) water. Such structural similarity supports theories that predict a similar sharp transition in pure water under pressure if ice crystallization could be suppressed.

Liquid Crystal Phases of Colloidal Platelets and their Use as Nanocomposite Templates

NARCIS (Netherlands)

Mourad, M.C.D.|info:eu-repo/dai/nl/304837563

2009-01-01

This thesis explores the gelation and liquid crystal phase behavior of colloidal dispersions of platelike particles as well as the use of such dispersions for the generation of nanocomposites. We report on the sol-gel, sol-glass and liquid crystal phase transitions of positively charged colloidal

Description of Adsorption in Liquid Chromatography under Nonideal Conditions.

Science.gov (United States)

Ortner, Franziska; Ruppli, Chantal; Mazzotti, Marco

2018-05-15

A thermodynamically consistent description of binary adsorption in reversed-phase chromatography is presented, accounting for thermodynamic nonidealities in the liquid and adsorbed phases. The investigated system involves the adsorbent Zorbax 300SB-C18, as well as phenetole and 4- tert-butylphenol as solutes and methanol and water as inert components forming the eluent. The description is based on adsorption isotherms, which are a function of the liquid-phase activities, to account for nonidealities in the liquid phase. Liquid-phase activities are calculated with a UNIQUAC model established in this work, based on experimental phase equilibrium data. The binary interaction in the adsorbed phase is described by the adsorbed solution theory, assuming an ideal (ideal adsorbed solution theory) or real (real adsorbed solution theory) adsorbed phase. Implementation of the established adsorption model in a chromatographic code achieves a quantitative description of experimental elution profiles, with feed compositions exploiting the entire miscible region, and involving a broad range of different eluent compositions (methanol/water). The quantitative agreement of the model and experimental data serves as a confirmation of the underlying physical (thermodynamic) concepts and of their applicability to a broad range of operating conditions.

High-performance liquid chromatographic separations of stereoisomers of chiral basic agrochemicals with polysaccharide-based chiral columns and polar organic mobile phases.

Science.gov (United States)

Matarashvili, Iza; Shvangiradze, Iamze; Chankvetadze, Lali; Sidamonidze, Shota; Takaishvili, Nino; Farkas, Tivadar; Chankvetadze, Bezhan

2015-12-01

The separation of the stereoisomers of 23 chiral basic agrochemicals was studied on six different polysaccharide-based chiral columns in high-performance liquid chromatography with various polar organic mobile phases. Along with the successful separation of analyte stereoisomers, emphasis was placed on the effect of the chiral selector and mobile phase composition on the elution order of stereoisomers. The interesting phenomenon of reversal of enantiomer/stereoisomer elution order function of the polysaccharide backbone (cellulose or amylose), type of derivative (carbamate or benzoate), nature, and position of the substituent(s) in the phenylcarbamate moiety (methyl or chloro) and the nature of the mobile phase was observed. For several of the analytes containing two chiral centers all four stereoisomers were resolved with at least one chiral selector/mobile phase combination. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of Poly(styrene-block-t-butyl methacrylate) Copolymers by Various Liquid Chromatography Techniques

Science.gov (United States)

Šmigovec Ljubič, Tina; Pahovnik, David; Žigon, Majda; Žagar, Ema

2012-01-01

The separation of a mixture of three poly(styrene-block-t-butyl methacrylate) copolymers (PS-b-PtBMA), consisting of polystyrene (PS) blocks of similar length and t-butyl methacrylate (PtBMA) blocks of different lengths, was performed using various chromatographic techniques, that is, a gradient liquid chromatography on reversed-phase (C18 and C8) and normal-phase columns, a liquid chromatography under critical conditions for polystyrene as well as a fully automated two-dimensional liquid chromatography that separates block copolymers by chemical composition in the first dimension and by molar mass in the second dimension. The results show that a partial separation of the mixture of PS-b-PtBMA copolymers can be achieved only by gradient liquid chromatography on reversed-phase columns. The coelution of the two block copolymers is ascribed to a much shorter PtBMA block length, compared to the PS block, as well as a small difference in the length of the PtBMA block in two of these copolymers, which was confirmed by SEC-MALS and NMR spectroscopy. PMID:22489207

The reversal phase of the bone-remodeling cycle

DEFF Research Database (Denmark)

Delaisse, Jean-Marie

2014-01-01

coincides with decreased osteoblast recruitment and impaired initiation of bone formation, that is, uncoupling. Overall, this review stresses that coupling does not only depend on molecules able to activate osteogenesis, but that it also demands the presence of osteoprogenitors and ordered cell......The reversal phase couples bone resorption to bone formation by generating an osteogenic environment at remodeling sites. The coupling mechanism remains poorly understood, despite the identification of a number of 'coupling' osteogenic molecules. A possible reason is the poor attention...

Solid-phase extraction combined with dispersive liquid-liquid microextraction and chiral liquid chromatography-tandem mass spectrometry for the simultaneous enantioselective determination of representative proton-pump inhibitors in water samples.

Science.gov (United States)

Zhao, Pengfei; Deng, Miaoduo; Huang, Peiting; Yu, Jia; Guo, Xingjie; Zhao, Longshan

2016-09-01

This report describes, for the first time, the simultaneous enantioselective determination of proton-pump inhibitors (PPIs-omeprazole, lansoprazole, pantoprazole, and rabeprazole) in environmental water matrices based on solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and chiral liquid chromatography-tandem mass spectrometry. The optimized results of SPE-DLLME were obtained with PEP-2 column using methanol-acetonitrile (1/1, v/v) as elution solvent, dichloroethane, and acetonitrile as extractant and disperser solvent, respectively. The separation and determination were performed using reversed-phase chromatography on a cellulose chiral stationary phase, a Chiralpak IC (250 mm × 4.6 mm, 5 μm) column, under isocratic conditions at 0.6 mL min(-1) flow rate. The analytes were detected in multiple reaction monitoring (MRM) mode by triple quadrupole mass spectrometry. Isotopically labeled internal standards were used to compensate matrix interferences. The method provided enrichment factors of around 500. Under optimal conditions, the mean recoveries for all eight enantiomers from the water samples were 89.3-107.3 % with 0.9-10.3 % intra-day RSD and 2.3-8.1 % inter-day RSD at 20 and 100 ng L(-1) levels. Correlation coefficients (r (2)) ≥ 0.999 were achieved for all enantiomers within the range of 2-500 μg L(-1). The method detection and quantification limits were at very low levels, within the range of 0.67-2.29 ng L(-1) and 2.54-8.68 ng L(-1), respectively. This method was successfully applied to the determination of the concentrations and enantiomeric fractions of the targeted analytes in wastewater and river water, making it applicable to the assessment of the enantiomeric fate of PPIs in the environment. Graphical Abstract Simultaneous enantioselective determination of representative proton-pump inhibitors in water samples.

A numerical study of aerosol influence on mixed-phase stratiform clouds through modulation of the liquid phase

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G. de Boer

2013-02-01

Full Text Available Numerical simulations were carried out in a high-resolution two-dimensional framework to increase our understanding of aerosol indirect effects in mixed-phase stratiform clouds. Aerosol characteristics explored include insoluble particle type, soluble mass fraction, influence of aerosol-induced freezing point depression and influence of aerosol number concentration. Simulations were analyzed with a focus on the processes related to liquid phase microphysics, and ice formation was limited to droplet freezing. Of the aerosol properties investigated, aerosol insoluble mass type and its associated freezing efficiency was found to be most relevant to cloud lifetime. Secondary effects from aerosol soluble mass fraction and number concentration also alter cloud characteristics and lifetime. These alterations occur via various mechanisms, including changes to the amount of nucleated ice, influence on liquid phase precipitation and ice riming rates, and changes to liquid droplet nucleation and growth rates. Alteration of the aerosol properties in simulations with identical initial and boundary conditions results in large variability in simulated cloud thickness and lifetime, ranging from rapid and complete glaciation of liquid to the production of long-lived, thick stratiform mixed-phase cloud.

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

International Nuclear Information System (INIS)

Catalá-Icardo, M.; Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C.; Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G.; Herrero-Martínez, J.M.

2017-01-01

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch"®), or mixtures of H_2O_2 and H_2SO_4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Catalá-Icardo, M., E-mail: mocaic@qim.upv.es [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C. [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G. [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain); Herrero-Martínez, J.M., E-mail: jmherrer@uv.es [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain)

2017-04-01

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch{sup ®}), or mixtures of H{sub 2}O{sub 2} and H{sub 2}SO{sub 4}, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

Determination of adrenaline, noradrenaline and corticosterone in rodent blood by ion pair reversed phase UHPLC-MS/MS.

Science.gov (United States)

Bergh, Marianne Skov-Skov; Bogen, Inger Lise; Andersen, Jannike Mørch; Øiestad, Åse Marit Leere; Berg, Thomas

2018-01-01

A novel ion pair reversed phase ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of the stress hormones adrenaline, noradrenaline and corticosterone in rodent blood was developed and fully validated. Separations were performed on an Acquity HSS T3 column (2.1mm i.d.×100mm, 1.8μm) with gradient elution and a runtime of 5.5min. The retention of adrenaline and noradrenaline was substantially increased by employing the ion pair reagent heptafluorobutyric acid (HFBA). Ion pair reagents are usually added to the mobile phase only, but we demonstrate for the first time that including HFBA to the sample reconstitution solvent as well, has a major impact on the chromatography of these compounds. The stability of adrenaline and corticosterone in rodent blood was investigated using the surrogate analytes adrenaline-d 3 and corticosterone-d 8 . The applicability of the described method was demonstrated by measuring the concentration of stress hormones in rodent blood samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Séparations par changement de phase. Etude et représentation des équilibres liquide-vapeur Separation by Phase Hange. Study and Computing Liquid-Vapor Equilibria

Directory of Open Access Journals (Sweden)

Asselineau L.

2006-11-01

Full Text Available Pour concevoir et optimiser les principales opérations de séparation (particulièrement les distillations avec ou sans solvant et l'extraction liquide-liquide on doit disposer de méthodes de corrélation ou, mieux, de prédiction des équilibres entre phases. A basse pression, et pour les mélanges d'hydrocarbures, les résultats présentés permettent la prévision des coefficients d'équilibre, même pour les séparations les plus délicates. En présence de constituants polaires, les données expérimentales d'équilibre liquide-liquide et liquide-vapeur de mélanges binaires et ternaires peuvent être simultanément corrélées dans le but de simuler et d'optimiser les distillations azéotropiques ou extractives. Sous haute pression, et particulièrement aux abords immédiats du point critique, le choix d'une équation d'état conduit à un traitement unitaire des phases en présence et permet, en particulier, la prédiction du lieu des points critiques des mélanges d'hydrocarbures et la corrélation de ce lieu en présence de solvants polaires. To determine and optimize the main separation operations (in particular distillations with or without a solvent, and liquid-liquid extraction correlation methods must be available or, better yet, methods of predicting phase equilibria. At low pressure and for hydrocarbon mixtures, the results described make the prediction of equilibrium coefficients possible, even for the most delicate separation. In the presence of polar constituents, the experimental data for the liquid-liquid and liquid-vapor equilibrium of binary and ternary mixtures can be simultaneously correlaten so as to simulate and optimize azeotropic or extractive distillations. Under high pressure and especially in the immediate vicinityof the critical point, the choice of an equation of state leads ta a unit treatment of the phases present and, in particular, makes it possible to predict the location of critical points in hydrocarbon

Group theoretical arguments on the Landau theory of second-order phase transitions applied to the phase transitions in some liquid crystals

International Nuclear Information System (INIS)

Rosciszewski, K.

1979-01-01

The phase transitions between liquids and several of the simplest liquid crystalline phases (nematic, cholesteric, and the simplest types of smectic A and smectic C) were studied from the point of view of the group-theoretical arguments of Landau theory. It was shown that the only possible candidates for second-order phase transitions are those between nematic and smectic A, between centrosymmetric nematic and smectic C and between centrosymmetric smectic A and smectic C. Simple types of density functions for liquid crystalline phases are proposed. (author)

Liquid-Liquid Phase Separation in Model Nuclear Waste Glasses: A Solid-State Double-Resonance NMR Study

Energy Technology Data Exchange (ETDEWEB)

Martineau, Ch.; Michaelis, V.K.; Kroeker, S. [Univ Manitoba, Dept Chem, Winnipeg, MB R3T 2N2 (Canada); Schuller, S. [CEA Valrho Marcoule, LDMC, SECM, DTCD, DEN, F-30207 Bagnols Sur Ceze (France)

2010-07-01

Double-resonance nuclear magnetic resonance (NMR) techniques are used in addition to single-resonance NMR experiments to probe the degree of mixing between network-forming cations Si and B, along with the modifier cations Cs{sup +} and Na{sup +} in two molybdenum-bearing model nuclear waste glasses. The double-resonance experiments involving {sup 29}Si in natural abundance are made possible by the implementation of a CPMG pulse-train during the acquisition period of the usual REDOR experiments. For the glass with lower Mo content, the NMR results show a high degree of Si-B mixing, as well as an homogeneous distribution of the cations within the borosilicate network, characteristic of a non-phase-separated glass. For the higher-Mo glass, a decrease of B-Si(Q{sup 4}) mixing is observed, indicating phase separation. {sup 23}Na and {sup 133}Cs NMR results show that although the Cs{sup +} cations, which do not seem to be influenced by the molybdenum content, are spread within the borate network, there is a clustering of the Na{sup +} cations, very likely around the molybdate units. The segregation of a Mo-rich region with Na{sup +} cations appears to shift the bulk borosilicate glass composition toward the metastable liquid liquid immiscibility region and induce additional phase separation. Although no crystallization is observed in the present case, this liquid liquid phase separation is likely to be the first stage of crystallization that can occur at higher Mo loadings or be driven by heat treatment. From this study emerges a consistent picture of the nature and extent of such phase separation phenomena in Mo-bearing glasses, and demonstrates the potential of double-resonance NMR methods for the investigation of phase separation in amorphous materials. (authors)

Correlations between phase behaviors and ionic conductivities of (ionic liquid + alcohol) systems

International Nuclear Information System (INIS)

Park, Nam Ku; Bae, Young Chan

2010-01-01

To understand the basic properties of ionic liquids (ILs), we examined the phase behavior and ionic conductivity characteristics using various compositions of different ionic liquids (1-ethyl-3-methylimidazolium hexafluorophosphate [emim] [PF6] and 1-benzyl-3-methylimidazolium hexafluorophosphate [bzmim] [PF6]) in several different alcohols (ethanol, propanol, 1-butanol, 2-butanol, and hexanol). We conducted a systematic study of the impact of different factors on the phase behavior of imidazolium-based ionic liquids in alcohols. Using a new experimental method with a liquid electrolyte system, we observed that the ionic conductivity of the ionic liquid/alcohol was sensitive to the surrounding temperature. We employed Chang et al.'s thermodynamic model [Chang et al. (1997, 1998) ] based on the lattice model. The obtained co-ordinated unit parameter from this model was used to describe the phase behavior and ionic conductivities of the given system. Good agreement with experimental data of various alcohol and ILs systems was obtained in the range of interest.

Reversed-phase single drop microextraction followed by high-performance liquid chromatography with fluorescence detection for the quantification of synthetic phenolic antioxidants in edible oil samples.

Science.gov (United States)

Farajmand, Bahman; Esteki, Mahnaz; Koohpour, Elham; Salmani, Vahid

2017-04-01

The reversed-phase mode of single drop microextraction has been used as a preparation method for the extraction of some phenolic antioxidants from edible oil samples. Butylated hydroxyl anisole, tert-butylhydroquinone and butylated hydroxytoluene were employed as target compounds for this study. High-performance liquid chromatography followed by fluorescence detection was applied for final determination of target compounds. The most interesting feature of this study is the application of a disposable insulin syringe with some modification for microextraction procedure that efficiently improved the volume and stability of the solvent microdrop. Different parameters such as the type and volume of solvent, sample stirring rate, extraction temperature, and time were investigated and optimized. Analytical performances of the method were evaluated under optimized conditions. Under the optimal conditions, relative standard deviations were between 4.4 and 10.2%. Linear dynamic ranges were 20-10 000 to 2-1000 μg/g (depending on the analytes). Detection limits were 5-670 ng/g. Finally, the proposed method was successfully used for quantification of the antioxidants in some edible oil samples prepared from market. Relative recoveries were achieved from 88 to 111%. The proposed method had a simplicity of operation, low cost, and successful application for real samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid-phase turbulence measurements in air-water two-phase flows over a wide range of void fractions

Energy Technology Data Exchange (ETDEWEB)

Zhou, Xinquan [Nuclear Engineering Program, Department of Mechanical and Aerospace Engineering, The Ohio State University, 201 W. 19th Ave., Columbus, OH 43210 (United States); Sun, Xiaodong, E-mail: sun.200@osu.edu [Nuclear Engineering Program, Department of Mechanical and Aerospace Engineering, The Ohio State University, 201 W. 19th Ave., Columbus, OH 43210 (United States); Liu, Yang [Nuclear Engineering Program, Department of Mechanical Engineering, Virginia Tech, 635 Prices Fork Road, Blacksburg, VA 24061 (United States)

2016-12-15

This paper focuses on liquid-phase turbulence measurements in air-water two-phase flows over a wide range of void fractions and flow regimes, spanning from bubbly, cap-bubbly, slug, to churn-turbulent flows. The measurements have been conducted in two test facilities, the first one with a circular test section and the second one with a rectangular test section. A particle image velocimetry-planar laser-induced fluorescence (PIV-PLIF) system was used to acquire local liquid-phase turbulence information, including the time-averaged velocity and velocity fluctuations in the streamwise and spanwise directions, and Reynolds stress. An optical phase separation method using fluorescent particles and optical filtration technique was adopted to extract the liquid-phase velocity information. An image pre-processing scheme was imposed on the raw PIV images acquired to remove noise due to the presence of bubble residuals and optically distorted particles in the raw PIV images. Four-sensor conductivity probes and high-speed images were also used to acquire the gas-phase information, which was aimed to understand the flow interfacial structure. The highest area-averaged void fraction covered in the measurements for the circular and rectangular test sections was about 40%.

Liquid-phase turbulence measurements in air-water two-phase flows over a wide range of void fractions

International Nuclear Information System (INIS)

Zhou, Xinquan; Sun, Xiaodong; Liu, Yang

2016-01-01

This paper focuses on liquid-phase turbulence measurements in air-water two-phase flows over a wide range of void fractions and flow regimes, spanning from bubbly, cap-bubbly, slug, to churn-turbulent flows. The measurements have been conducted in two test facilities, the first one with a circular test section and the second one with a rectangular test section. A particle image velocimetry-planar laser-induced fluorescence (PIV-PLIF) system was used to acquire local liquid-phase turbulence information, including the time-averaged velocity and velocity fluctuations in the streamwise and spanwise directions, and Reynolds stress. An optical phase separation method using fluorescent particles and optical filtration technique was adopted to extract the liquid-phase velocity information. An image pre-processing scheme was imposed on the raw PIV images acquired to remove noise due to the presence of bubble residuals and optically distorted particles in the raw PIV images. Four-sensor conductivity probes and high-speed images were also used to acquire the gas-phase information, which was aimed to understand the flow interfacial structure. The highest area-averaged void fraction covered in the measurements for the circular and rectangular test sections was about 40%.