A Novel High Performance Liquid Chromatographic Method for Simultaneous Determination of Ceftriaxone and Sulbactam in Sulbactomax

PubMed Central

Shrivastava, Sanjay Mohan; Singh, Rajkumar; Tariq, Abu; Siddiqui, Masoom Raza; Yadav, Jitendar; Negi, P. S.; Chaudhary, Manu

2009-01-01

An isocratic liquid chromatographic method with UV detection at 220 nm is described for simultaneous determination of ceftriaxone sodium and sulbactam sodium in Sulbactomax. Chromatographic separation of two drugs was achieved on a Hypersil ODS C-18 column using a mobile phase consisting of a binary mixture of acetonitrile and tetrabutyl ammonium hydroxide adjusted to pH7.0 with orthophosphoric acid in ratio 70:30. The developed Liquid Chromatographic method offers symmetric peak shape, good resolution and reasonable retention time for both drugs. Linearity, accuracy and precision were found to be acceptable over the concentration range of 125-750 ppm for ceftriaxone sodium and 62.5-375 ppm for sulbactam sodium. The LC method can be used for the quality control of formulated products containing ceftriaxone and sulbactam. PMID:23675112

Biodegradation kinetics of dissolved organic matter chromatographic fractions in an intermittent river

NASA Astrophysics Data System (ADS)

Catalán, N.; Casas-Ruiz, J. P.; von Schiller, D.; Proia, L.; Obrador, B.; Zwirnmann, E.; Marcé, R.

2017-01-01

Controls on the degradation of dissolved organic matter (DOM) are complex but key to understand the role of freshwaters in the carbon cycle. Both the origin and previous degradation history have been suggested to determine DOM reactivity, but it is still a major challenge to understand the links between DOM composition and biodegradation kinetics. An appropriate context to study these links are intermittent rivers, as summer drought naturally diversifies DOM sources and sinks. Here we investigated the biodegradation kinetics of DOM in the main aquatic environments present in a temporary river. During dark incubations we traced the dynamics of bulk DOM and its main chromatographic fractions defined using LC-OCD: high molecular weight substances (HMWS), low molecular weight substances (LMWS), and humic substances and building blocks. Bulk DOM decay patterns were successfully fitted to the reactivity continuum (RC) biodegradation model. The RC parameters depicted running waters as the sites presenting a more reactive DOM, and temporary pools, enriched in leaf litter, as the ones with slowest DOM decay. The decay patterns of each DOM fraction were consistent throughout sites. LMWS and HMWS decayed in all cases and could be modeled using the RC model. Notably, the dynamics of LMWS controlled the bulk DOM kinetics. We discuss the mechanistic basis for the chromatographic fractions' kinetics during biodegradation and the implications that preconditioning and summer drought can have for DOM biodegradation in intermittent rivers.

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

PubMed

Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

2014-06-13

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

Determinations of gas-liquid partition coefficients using capillary chromatographic columns. Alkanols in squalane.

PubMed

Tascon, Marcos; Romero, Lílian M; Acquaviva, Agustín; Keunchkarian, Sonia; Castells, Cecilia

2013-06-14

This study focused on an investigation into the experimental quantities inherent in the determination of partition coefficients from gas-liquid chromatographic measurements through the use of capillary columns. We prepared several squalane - (2,6,10,15,19,23-hexamethyltetracosane) - containing columns with very precisely known phase ratios and determined solute retention and hold-up times at 30, 40, 50 and 60°C. We calculated infinite dilution partition coefficients from the slopes of the linear regression of retention factors as a function of the reciprocal of the phase ratio by means of fundamental chromatographic equations. In order to minimize gas-solid and liquid-solid interface contributions to retention, the surface of the capillary inner wall was pretreated to guarantee a uniform coat of stationary phase. The validity of the proposed approach was first tested by estimating the partition coefficients of n-alkanes between n-pentane and n-nonane, for which compounds data from the literature were available. Then partition coefficients of sixteen aliphatic alcohols in squalane were determined at those four temperatures. We deliberately chose these highly challenging systems: alcohols in the reference paraffinic stationary phase. These solutes exhibited adsorption in the gas-liquid interface that contributed to retention. The corresponding adsorption constant values were estimated. We fully discuss here the uncertainties associated with each experimental measurement and how these fundamental determinations can be performed precisely by circumventing the main drawbacks. The proposed strategy is reliable and much simpler than the classical chromatographic method employing packed columns. Copyright © 2013 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic method for guanylhydrazone compounds.

PubMed

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

1996-01-12

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

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

PubMed

Simonaitis, R A; Cail, R S

1975-09-01

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

QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

PubMed

Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

2016-06-01

The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

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

PubMed

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

2015-08-01

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

Liquid chromatographic characterization of PMR-15 resin and prepreg

NASA Technical Reports Server (NTRS)

Reed, K. E.

1980-01-01

A liquid chromatographic method has been developed capable of providing a chemical fingerprint of PMR-15 resin solutions and prepreg. The amounts of two of the monomers can be quantified so their experimentally determined molar ratio can be compared to the formulated one. Only the monomers were detected in fresh resin solution, whereas several additional components, resulting from an association or reaction between the norbornenyl endcap and the amine, were detected in a resin solution aged for three days. Two commercial prepregs exhibited fingerprints similar to that of laboratory material, but three others contained additional components corresponding to higher esters and nadimides.

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

PubMed

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

2016-05-01

This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at -4°C. Contaminant peak was detected in methanol stored in polypropylene microcentrifuge tubes using UFLC analysis. The contaminant peak detected was prominent, sharp detectable at 9.176 ± 0.138 min on a Waters 250-4.6 mm, 4 μ, Nova-Pak C18 column with mobile phase consisting of methanol:water (70:30). It was evident from the study that long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peak. Further, this may mislead in future reporting an unnatural compound by researchers. Long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peakContamination peak with higher area under the curve (609993) was obtained in ultra-flow liquid chromatographic run for methanol stored in PP microcentrifuge tubesContamination peak was detected at retention time 9.113 min with a lambda max of 220.38 nm and 300 mAU intensity on the given chromatographic conditionsGlass vials serve better option over PP microcentrifuge tubes for storing biological samples. Abbreviations used: UFLC: Ultra Flow Liquid Chromatography; LC: Liquid Chromatography; MS: Mass spectrometry; AUC: Area Under Curve.

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

PubMed

Cserháti, T; Forgács, E

2001-11-30

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

High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

EPA Science Inventory

A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

EPA Science Inventory

High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) was obtained on polysaccharide enantioselective HPLC columns using alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, fonofos, fenamiph...

High-performance liquid chromatographic determination of the beta2-selective adrenergic agonist fenoterol in human plasma after fluorescence derivatization.

PubMed

Kramer, S; Blaschke, G

2001-02-10

A sensitive high-performance liquid chromatographic method has been developed for the determination of the beta2-selective adrenergic agonist fenoterol in human plasma. To improve the sensitivity of the method, fenoterol was derivatized with N-(chloroformyl)-carbazole prior to HPLC analysis yielding highly fluorescent derivatives. The assay involves protein precipitation with acetonitrile, liquid-liquid-extraction of fenoterol from plasma with isobutanol under alkaline conditions followed by derivatization with N-(chloroformyl)-carbazole. Reversed-phase liquid chromatographic determination of the fenoterol derivative was performed using a column-switching system consisting of a LiChrospher 100 RP 18 and a LiChrospher RP-Select B column with acetonitrile, methanol and water as mobile phase. The limit of quantitation in human plasma was 376 pg fenoterol/ml. The method was successfully applied for the assay of fenoterol in patient plasma.

Liquid-chromatographic determination of cephalosporins and chloramphenicol in serum.

PubMed

Danzer, L A

1983-05-01

A "high-performance" liquid-chromatographic technique involving a radial compression module is used for measuring chloramphenicol and five cephalosporin antibiotics: cefotaxime, cefoxitin, cephapirin, and cefamandol. Serum proteins are precipitated with acetonitrile solution containing 4'-nitroacetanilide as the internal standard. The drugs are eluted with a mobile phase of methanol/acetate buffer (30/70 by vol), pH 5.5. Absorbance of the cephalosporins is monitored at 254 nm. Standard curves are linear to at least 100 mg/L. The absorbance of chloramphenicol is monitored at 254 nm and 280 nm, and its standard curve is linear to at least 50 mg/L. The elution times for various other drugs were also determined, to check for potential interferents.

Two-Dimensional Offline Chromatographic Fractionation for the Characterization of Humic-Like Substances in Atmospheric Aerosol Particles.

PubMed

Spranger, Tobias; van Pinxteren, Dominik; Herrmann, Hartmut

2017-05-02

Organic carbon in atmospheric particles comprises a large fraction of chromatographically unresolved compounds, often referred to as humic-like substances (HULIS), which influence particle properties and impact climate, human health, and ecosystems. To better understand its composition, a two-dimensional (2D) offline method combining size-exclusion (SEC) and reversed-phase liquid chromatography (RP-HPLC) using a new spiked gradient profile is presented. It separates HULIS into 55 fractions of different size and polarity, with estimated ranges of molecular weight and octanol/water partitioning coefficient (log P) from 160-900 g/mol and 0.2-3.3, respectively. The distribution of HULIS within the 2D size versus polarity space is illustrated with heat maps of ultraviolet absorption at 254 nm. It is found to strongly differ in a small example set of samples from a background site near Leipzig, Germany. In winter, the most intense signals were obtained for the largest molecules (>520 g/mol) with low polarity (log P ∼ 1.9), whereas in summer, smaller (225-330 g/mol) and more polar (log P ∼ 0.55) molecules dominate. The method reveals such differences in HULIS composition in a more detailed manner than previously possible and can therefore help to better elucidate the sources of HULIS in different seasons or at different sites. Analyzing Suwannee river fulvic acid as a common HULIS surrogate shows a similar polarity range, but the sizes are clearly larger than those of atmospheric HULIS.

Isolation and recovery of selected polybrominated diphenyl ethers from human serum and sheep serum: coupling reversed-phase solid-phase disk extraction and liquid-liquid extraction techniques with a capillary gas chromatographic electron capture negative ion mass spectrometric determinative technique.

PubMed

Loconto, Paul R; Isenga, David; O'Keefe, Michael; Knottnerus, Mark

2008-01-01

Polybrominated diphenyl ethers (PBDEs) are isolated and recovered with acceptable percent recoveries from human serum via liquid-liquid extraction and column chromatographic cleanup and fractionation with quantitation using capillary gas chromatography-mass spectrometry with electron capture negative ion and selected ion monitoring. PBDEs are found in unspiked serum. An alternative sample preparation approach is developed using sheep serum that utilizes a formic acid pre-treatment followed by reversed-phase solid-phase disk extraction and normal-phase solid-phase cleanup using acidified silica gel that yields>50% recoveries. When these percent recoveries are combined with a minimized phase ratio for human serum and very low instrument detection limits, method detection limits below 500 parts-per-trillion are realized.

High-performance liquid chromatographic method for potency determination of amoxicillin in commercial preparations and for stability studies.

PubMed Central

Hsu, M C; Hsu, P W

1992-01-01

A reversed-phase column liquid chromatographic method was developed for the assay of amoxicillin and its preparations. The linear calibration range was 0.2 to 2.0 mg/ml (r = 0.9998), and recoveries were generally greater than 99%. The high-performance liquid chromatographic assay results were compared with those obtained from a microbiological assay of bulk drug substance and capsule, injection, and granule formulations containing amoxicillin and degraded amoxicillin. At the 99% confidence level, no significant intermethod differences were noted for the paired results. Commercial formulations were also analyzed, and the results obtained by the proposed method closely agreed with those found by the microbiological method. The results indicated that the proposed method is a suitable substitute for the microbiological method for assays and stability studies of amoxicillin preparations. PMID:1416827

A new analytical method for quantification of olive and palm oil in blends with other vegetable edible oils based on the chromatographic fingerprints from the methyl-transesterified fraction.

PubMed

Jiménez-Carvelo, Ana M; González-Casado, Antonio; Cuadros-Rodríguez, Luis

2017-03-01

A new analytical method for the quantification of olive oil and palm oil in blends with other vegetable edible oils (canola, safflower, corn, peanut, seeds, grapeseed, linseed, sesame and soybean) using normal phase liquid chromatography, and applying chemometric tools was developed. The procedure for obtaining of chromatographic fingerprint from the methyl-transesterified fraction from each blend is described. The multivariate quantification methods used were Partial Least Square-Regression (PLS-R) and Support Vector Regression (SVR). The quantification results were evaluated by several parameters as the Root Mean Square Error of Validation (RMSEV), Mean Absolute Error of Validation (MAEV) and Median Absolute Error of Validation (MdAEV). It has to be highlighted that the new proposed analytical method, the chromatographic analysis takes only eight minutes and the results obtained showed the potential of this method and allowed quantification of mixtures of olive oil and palm oil with other vegetable oils. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

PubMed

Barker, S A; Long, A R

1994-01-01

The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

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

PubMed

Beasley, T H; Ziegler, H W

1977-12-01

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

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

PubMed Central

Larsen, K.K.; Wielandt, D.; Schiller, M.; Bizzarro, M.

2016-01-01

Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of these species can result in incomplete Cr recovery during chromatographic purification. Because of large mass-dependent inter-species isotope fractionation, incomplete recovery can affect the accuracy of high-precision Cr isotope analysis. Here, we demonstrate widely differing cation distribution coefficients of Cr(III)-species (Cr3+, CrCl2+ and CrCl2+) with equilibrium mass-dependent isotope fractionation spanning a range of ~1‰/amu and consistent with theory. The heaviest isotopes partition into Cr3+, intermediates in CrCl2+ and the lightest in CrCl2+/CrCl3°. Thus, for a typical reported loss of ~25% Cr (in the form of Cr3+) through chromatographic purification, this translates into 185 ppm/amu offset in the stable Cr isotope ratio of the residual sample. Depending on the validity of the mass-bias correction during isotope analysis, this further results in artificial mass-independent effects in the mass-bias corrected 53Cr/52Cr (μ53 Cr* of 5.2 ppm) and 54Cr/52Cr (μ54Cr* of 13.5 ppm) components used to infer chronometric and nucleosynthetic information in meteorites. To mitigate these fractionation effects, we developed strategic chemical sample pre-treatment procedures that ensure high and reproducible Cr recovery. This is achieved either through 1) effective promotion of Cr3+ by >5 days exposure to HNO3 —H2O2 solutions at room temperature, resulting in >~98% Cr recovery for most types of sample matrices tested using a cationic chromatographic retention strategy, or 2) formation of Cr(III)-Cl complexes through exposure to concentrated HCl at high temperature (>120 °C) for several hours, resulting in >97.5% Cr recovery using a chromatographic elution strategy that

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

PubMed

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

2014-09-12

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

Determination of high-molecular weight polycyclic aromatic hydrocarbons in high performance liquid chromatography fractions of coal tar standard reference material 1597a via solid-phase nanoextraction and laser-excited time-resolved Shpol'skii spectroscopy

PubMed Central

Wilson, Walter B.; Alfarhani, Bassam; Moore, Anthony F. T.; Bisson, Cristina; Wise, Stephen A.; Campiglia, Andres D.

2016-01-01

This article presents an alternative approach for the analysis of high molecular weight – polycyclic aromatic hydrocarbons (HMW-PAHs) with molecular mass 302 Da in complex environmental samples. This is not a trivial task due to the large number of molecular mass 302 Da isomers with very similar chromatographic elution times and similar, possibly even virtually identical, mass fragmentation patterns. The method presented here is based on 4.2 K laser-excited time-resolved Shpol'skii spectroscopy, a high resolution spectroscopic technique with the appropriate selectivity for the unambiguous determination of PAHs with the same molecular mass. The potential of this approach is demonstrated here with the analysis of a coal tar standard reference material (SRM) 1597a. Liquid chromatography fractions were submitted to the spectroscopic analysis of five targeted isomers, namely dibenzo[a,l]pyrene, dibenzo[a,e]pyrene, dibenzo[a,i]pyrene, naphtho[2,3-a]pyrene and dibenzo[a,h]pyrene. Prior to analyte determination, the liquid chromatographic fractions were pre-concentrated with gold nanoparticles. Complete analysis was possible with microliters of chromatographic fractions and organic solvents. The limits of detection varied from 0.05 (dibenzo[a,l]pyrene) to 0.24 μg L−1 (dibenzo[a,e]pyrene). The excellent analytical figures of merit associated to its non-destructive nature, which provides ample opportunity for further analysis with other instrumental methods, makes this approach an attractive alternative for the determination of PAH isomers in complex environmental samples. PMID:26653471

Process for stabilization of coal liquid fractions

DOEpatents

Davies, Geoffrey; El-Toukhy, Ahmed

1987-01-01

Coal liquid fractions to be used as fuels are stabilized against gum formation and viscosity increases during storage, permitting the fuel to be burned as is, without further expensive treatments to remove gums or gum-forming materials. Stabilization is accomplished by addition of cyclohexanol or other simple inexpensive secondary and tertiary alcohols, secondary and tertiary amines, and ketones to such coal liquids at levels of 5-25% by weight with respect to the coal liquid being treated. Cyclohexanol is a particularly effective and cost-efficient stabilizer. Other stabilizers are isopropanol, diphenylmethanol, tertiary butanol, dipropylamine, triethylamine, diphenylamine, ethylmethylketone, cyclohexanone, methylphenylketone, and benzophenone. Experimental data indicate that stabilization is achieved by breaking hydrogen bonds between phenols in the coal liquid, thereby preventing or retarding oxidative coupling. In addition, it has been found that coal liquid fractions stabilized according to the invention can be mixed with petroleum-derived liquid fuels to produce mixtures in which gum deposition is prevented or reduced relative to similar mixtures not containing stabilizer.

Core-Shell in Liquid Chromatography: Application for Determining Sulphonamides in Feed and Meat Using Conventional Chromatographic Systems

PubMed Central

Armentano, Antonio; Summa, Simona; Magro, Sonia Lo; D’Antini, Pasquale; Palermo, Carmen; Muscarella, Marilena

2016-01-01

A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster. PMID:28217560

Microsomal epoxide hydrolase of rat liver. Purification and characterization of enzyme fractions with different chromatographic characteristics.

PubMed Central

Bulleid, N J; Graham, A B; Craft, J A

1986-01-01

Microsomal epoxide hydrolase was purified from rat liver, and different fractions of the purified enzyme, which varied in their contents of phospholipid, were obtained by ion-exchange chromatography. One fraction (A), which did not bind to CM-cellulose, had a high phospholipid content, and a second fraction (B), which was eluted from CM-cellulose at high ionic strength, had a low phospholipid content. Removal of most of the phospholipid from fraction A altered its chromatographic behaviour. When the delipidated material was re-applied to CM-cellulose, most of the enzyme bound to the cation-exchanger. The specific activities of all the fractions described (with styrene epoxide [(1,2-epoxyethyl)benzene] as substrate) were altered by adding the non-ionic detergent Lubrol PX or phospholipid. Lubrol PX inhibited enzyme activity, and phospholipid reversed this inhibition. The various enzyme fractions isolated appeared to be different forms of the same protein, as judged by their minimum Mr values and immunochemical properties. These results indicate that different fractions of epoxide hydrolase isolated by ion-exchange chromatography probably are not different isoenzyme forms. Images Fig. 2. Fig. 3. PMID:3082328

An inverse gas chromatographic methodology for studying gas-liquid mass transfer.

PubMed

Paloglou, A; Martakidis, K; Gavril, D

2017-01-13

A novel methodology of reversed flow inverse gas chromatography (RF-IGC) is presented. It permits the simultaneous determination of mass transfer coefficients across the gas liquid interface as well as the respective solubility parameters and thermodynamic functions of dissolution of gases into liquids. The standard deviation of the experimentally determined parameters is estimated for first time, which combined with the successful comparison of the values of the present parameters with other literature ones ascertain the reliability of the methodology. Another novelty of the present work is that the chromatographic sampling of the physicochemical phenomena is done without performing the usual flow reversals procedure. Vinyl chloride monomer's (VCM) interaction with various composition liquid foods: orange juice, milk and olive oil was used as model system. The present transfer rates are controlled by the gas film at lower temperatures, but at higher temperatures the resistances in both films tend to become equal. The found liquid diffusivity values express the total mass transfer from the gas phase into the liquid's bulk and they decrease with rising temperature, as the solubilities of gases in liquids do. Solubility, expressed by Henry's law constant and the mean values of interfacial thickness are of the same order of magnitude to literature ones. From the thermodynamic point of view, VCM dissolution in all liquids is accompanied by significant heat release and it is a slightly non-spontaneous process, near equilibrium, while the entropy change values are negative. Copyright © 2016 Elsevier B.V. All rights reserved.

Liquid chromatographic separation of zalcitabine and its stereoisomers.

PubMed

Scypinski, S; Ross, A J

1994-10-01

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

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

PubMed

Larsen, K K; Wielandt, D; Schiller, M; Bizzarro, M

2016-04-22

Chromatographic purification of chromium (Cr), which is required for high-precision isotope analysis, is complicated by the presence of multiple Cr-species with different effective charges in the acid digested sample aliquots. The differing ion exchange selectivity and sluggish reaction rates of these species can result in incomplete Cr recovery during chromatographic purification. Because of large mass-dependent inter-species isotope fractionation, incomplete recovery can affect the accuracy of high-precision Cr isotope analysis. Here, we demonstrate widely differing cation distribution coefficients of Cr(III)-species (Cr(3+), CrCl(2+) and CrCl2(+)) with equilibrium mass-dependent isotope fractionation spanning a range of ∼1‰/amu and consistent with theory. The heaviest isotopes partition into Cr(3+), intermediates in CrCl(2+) and the lightest in CrCl2(+)/CrCl3°. Thus, for a typical reported loss of ∼25% Cr (in the form of Cr(3+)) through chromatographic purification, this translates into 185 ppm/amu offset in the stable Cr isotope ratio of the residual sample. Depending on the validity of the mass-bias correction during isotope analysis, this further results in artificial mass-independent effects in the mass-bias corrected (53)Cr/(52)Cr (μ(53)Cr* of 5.2 ppm) and (54)Cr/(52)Cr (μ(54)Cr* of 13.5 ppm) components used to infer chronometric and nucleosynthetic information in meteorites. To mitigate these fractionation effects, we developed strategic chemical sample pre-treatment procedures that ensure high and reproducible Cr recovery. This is achieved either through 1) effective promotion of Cr(3+) by >5 days exposure to HNO3H2O2 solutions at room temperature, resulting in >∼98% Cr recovery for most types of sample matrices tested using a cationic chromatographic retention strategy, or 2) formation of Cr(III)-Cl complexes through exposure to concentrated HCl at high temperature (>120 °C) for several hours, resulting in >97.5% Cr recovery using a

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

PubMed

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

2011-01-01

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

LIQUID CHROMATOGRAPHIC DETERMINATION OF 5-(METHYLAMINO)-2-PHENYL-4-[3-(TRIFLUROMETHYL) PHENYL]-3-(2H)-FURANONE IN SOIL

EPA Science Inventory

A rapid, sensitive method is described for the determination of 5-(methylamino)-2-phenyl-4-[3-(trifluromethyl)phenyl]-3-(2H)-furanone RE-40885) concentrations in three soil types. he method consists of extraction of soil samples with methanol, filtration, liquid chromatographic s...

Quality evaluation of extracted ion chromatograms and chromatographic peaks in liquid chromatography/mass spectrometry-based metabolomics data.

PubMed

Zhang, Wenchao; Zhao, Patrick X

2014-01-01

Extracted ion chromatogram (EIC) extraction and chromatographic peak detection are two important processing procedures in liquid chromatography/mass spectrometry (LC/MS)-based metabolomics data analysis. Most commonly, the LC/MS technique employs electrospray ionization as the ionization method. The EICs from LC/MS data are often noisy and contain high background signals. Furthermore, the chromatographic peak quality varies with respect to its location in the chromatogram and most peaks have zigzag shapes. Therefore, there is a critical need to develop effective metrics for quality evaluation of EICs and chromatographic peaks in LC/MS based metabolomics data analysis. We investigated a comprehensive set of potential quality evaluation metrics for extracted EICs and detected chromatographic peaks. Specifically, for EIC quality evaluation, we analyzed the mass chromatographic quality index (MCQ index) and propose a novel quality evaluation metric, the EIC-related global zigzag index, which is based on an EIC's first order derivatives. For chromatographic peak quality evaluation, we analyzed and compared six metrics: sharpness, Gaussian similarity, signal-to-noise ratio, peak significance level, triangle peak area similarity ratio and the local peak-related local zigzag index. Although the MCQ index is suited for selecting and aligning analyte components, it cannot fairly evaluate EICs with high background signals or those containing only a single peak. Our proposed EIC related global zigzag index is robust enough to evaluate EIC qualities in both scenarios. Of the six peak quality evaluation metrics, the sharpness, peak significance level, and zigzag index outperform the others due to the zigzag nature of LC/MS chromatographic peaks. Furthermore, using several peak quality metrics in combination is more efficient than individual metrics in peak quality evaluation.

Multiresidue chromatographic method for the determination of macrolide residues in muscle by high-performance liquid chromatography with UV detection.

PubMed

Juhel-Gaugain, M; Anger, B; Laurentie, M

1999-01-01

A high-performance liquid chromatographic (HPLC) method for the simultaneous determination of tilmicosin, tylosin, spiramycin, and its major metabolite neospiramycin was developed that is suitable for porcine, bovine, and poultry muscles. Macrolide residues were extracted from muscle with acetonitrile, fat was removed by liquid-liquid extraction with isooctane, and the extract was then cleaned on Bond Elut C18 cartridges. The HPLC separation was performed on an Inertsil ODS3 C18 column (150 x 4 mm) with 0.05% trifluoroacetic acid-acetonitrile in a gradient mode. Two different chromatographic gradients were used for tilmicosin-tylosin and spiramycin-neospiramycin, and the detection wavelengths were 287 and 232 nm, respectively. The method was validated from 1/2 the maximum residue limit (MRL) to 4 times the MRL with pork muscle samples. Mean recoveries were 60, 63.5, 51, and 42% for tilmicosin, tylosin, spiramycin, and neospiramycin, respectively. The detection limits are 15 micrograms/kg for tilmicosin and tylosin, 30 micrograms/kg for spiramycin, and 25 micrograms/kg for neospiramycin. Linearity, precision, and accuracy of the method were also tested.

Comprehensive two-dimensional liquid chromatographic analysis of poloxamers.

PubMed

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

2016-04-15

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

Simple and rapid high-performance liquid chromatographic method for the determination of aspartame and its metabolites in foods.

PubMed

Gibbs, B F; Alli, I; Mulligan, C N

1996-02-23

A method for the determination of aspartame (N-L-alpha-aspartyl-L-phenylalanine methyl ester) and its metabolites, applicable on a routine quality assurance basis, is described. Liquid samples (diet Coke, 7-Up, Pepsi, etc.) were injected directly onto a mini-cartridge reversed-phase column on a high-performance liquid chromatographic system, whereas solid samples (Equal, hot chocolate powder, pudding, etc.) were extracted with water. Optimising chromatographic conditions resulted in resolved components of interest within 12 min. The by-products were confirmed by mass spectrometry. Although the method was developed on a two-pump HPLC system fitted with a diode-array detector, it is straightforward and can be transformed to the simplest HPLC configuration. Using a single-piston pump (with damper), a fixed-wavelength detector and a recorder/integrator, the degradation of products can be monitored as they decompose. The results obtained were in harmony with previously reported tedious methods. The method is simple, rapid, quantitative and does not involve complex, hazardous or toxic chemistry.

Quality evaluation of extracted ion chromatograms and chromatographic peaks in liquid chromatography/mass spectrometry-based metabolomics data

PubMed Central

2014-01-01

Background Extracted ion chromatogram (EIC) extraction and chromatographic peak detection are two important processing procedures in liquid chromatography/mass spectrometry (LC/MS)-based metabolomics data analysis. Most commonly, the LC/MS technique employs electrospray ionization as the ionization method. The EICs from LC/MS data are often noisy and contain high background signals. Furthermore, the chromatographic peak quality varies with respect to its location in the chromatogram and most peaks have zigzag shapes. Therefore, there is a critical need to develop effective metrics for quality evaluation of EICs and chromatographic peaks in LC/MS based metabolomics data analysis. Results We investigated a comprehensive set of potential quality evaluation metrics for extracted EICs and detected chromatographic peaks. Specifically, for EIC quality evaluation, we analyzed the mass chromatographic quality index (MCQ index) and propose a novel quality evaluation metric, the EIC-related global zigzag index, which is based on an EIC's first order derivatives. For chromatographic peak quality evaluation, we analyzed and compared six metrics: sharpness, Gaussian similarity, signal-to-noise ratio, peak significance level, triangle peak area similarity ratio and the local peak-related local zigzag index. Conclusions Although the MCQ index is suited for selecting and aligning analyte components, it cannot fairly evaluate EICs with high background signals or those containing only a single peak. Our proposed EIC related global zigzag index is robust enough to evaluate EIC qualities in both scenarios. Of the six peak quality evaluation metrics, the sharpness, peak significance level, and zigzag index outperform the others due to the zigzag nature of LC/MS chromatographic peaks. Furthermore, using several peak quality metrics in combination is more efficient than individual metrics in peak quality evaluation. PMID:25350128

Fractionalized Fermi liquids and exotic superconductivity in the Kitaev-Kondo lattice

NASA Astrophysics Data System (ADS)

Seifert, Urban F. P.; Meng, Tobias; Vojta, Matthias

2018-02-01

Fractionalized Fermi liquids (FL*) have been introduced as non-Fermi-liquid metallic phases, characterized by coexisting electron-like charge carriers and local moments which form a fractionalized spin liquid. Here we investigate a Kondo lattice model on the honeycomb lattice with Kitaev interactions among the local moments, a concrete model hosting FL* phases based on Kitaev's Z2 spin liquid. We characterize the FL* phases via perturbation theory, and we employ a Majorana-fermion mean-field theory to map out the full phase diagram. Most remarkably we find nematic triplet superconducting phases which mask the quantum phase transition between fractionalized and conventional Fermi liquid phases. Their pairing structure is inherited from the Kitaev spin liquid; i.e., superconductivity is driven by Majorana glue.

Lithium, magnesium and sulfur purification from seawater using an ion chromatograph with a fraction collector system for stable isotope measurements.

PubMed

Yoshimura, Toshihiro; Araoka, Daisuke; Tamenori, Yusuke; Kuroda, Junichiro; Kawahata, Hodaka; Ohkouchi, Naohiko

2018-01-05

We describe the mass descrimination and validation of an offline method for purification of Li, Mg and S with an ion chromatograph coupled to an automated fraction collector for use prior to stable isotope measurements. Significant sub-fraction mass fractionation was observed for both the Li and the Mg stable isotope ratios. The lighter Li and heavier Mg isotopes were preferentially retained by the column, resulting in 7 Li/ 6 Li and 26 Mg/ 24 Mg biases up to 85.8‰ and 0.95‰, respectively. The isotopic compositions of Li, Mg, and S separated from seawater were δ 7 Li L-SVEC  = +30.9‰, δ 26 Mg DSM3  = -0.83 ± 0.10‰, and δ 34 S VCDT  = +19.4 ± 0.6‰; each chromatographic peak was completely recovered, and the results were in good agreement with the published values regardless of whether or not chemical suppressor was used. The purification method enables multi-isotope analysis of a sample using various mass spectrometry techniques, such as multiple-collector inductively coupled plasma and thermal ionization mass spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

High-performance liquid chromatographic characterization of some medical plant extracts used in cosmetic formulas.

PubMed

Schulz, H; Albroscheit, G

1988-06-17

Rapid and reliable methods are presented for the characterization of biologically active and/or characteristic constituents in aqueous extracts of Hamamelis virginiana, Matricaria chamomilla, Achillea millefolium, Thymus vulgaris, Althaea officinalis and Cinchonia spp. Prior to high-performance liquid chromatographic (HPLC) separation a clean-up step was performed using a solid-phase extraction system. The purified extracts were analysed by HPLC coupled with a diode-array detector and a fluorescence detector. In some instances, previously unreported components of the aqueous plant extracts were found.

Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

PubMed

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

2006-01-01

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

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

PubMed

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

1980-02-01

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

Structural origin of fractional Stokes-Einstein relation in glass-forming liquids

NASA Astrophysics Data System (ADS)

Pan, Shaopeng; Wu, Z. W.; Wang, W. H.; Li, M. Z.; Xu, Limei

2017-01-01

In many glass-forming liquids, fractional Stokes-Einstein relation (SER) is observed above the glass transition temperature. However, the origin of such phenomenon remains elusive. Using molecular dynamics simulations, we investigate the break- down of SER and the onset of fractional SER in a model of metallic glass-forming liquid. We find that SER breaks down when the size of the largest cluster consisting of trapped atoms starts to increase sharply at which the largest cluster spans half of the simulations box along one direction, and the fractional SER starts to follows when the largest cluster percolates the entire system and forms 3-dimentional network structures. Further analysis based on the percolation theory also confirms that percolation occurs at the onset of the fractional SER. Our results directly link the breakdown of the SER with structure inhomogeneity and onset of the fraction SER with percolation of largest clusters, thus provide a possible picture for the break- down of SER and onset of fractional SER in glass-forming liquids, which is is important for the understanding of the dynamic properties in glass-forming liquids.

High-efficiency high performance liquid chromatographic analysis of red wine anthocyanins.

PubMed

de Villiers, André; Cabooter, Deirdre; Lynen, Frédéric; Desmet, Gert; Sandra, Pat

2011-07-22

The analysis of anthocyanins in natural products is of significant relevance in recent times due to the recognised health benefits associated with their consumption. In red grapes and wines in particular, anthocyanins are known to contribute important properties to the sensory (colour and taste), anti-oxidant- and ageing characteristics. However, the detailed investigation of the alteration of these compounds during wine ageing is hampered by the challenges associated with the separation of grape-derived anthocyanins and their derived products. High performance liquid chromatography (HPLC) is primarily used for this purpose, often in combination with mass spectrometric (MS) detection, although conventional HPLC methods provide incomplete resolution. We have previously demonstrated how on-column inter-conversion reactions are responsible for poor chromatographic efficiency in the HPLC analysis of anthocyanins, and how an increase in temperature and decrease in particle size may improve the chromatographic performance. In the current contribution an experimental configuration for the high efficiency analysis of anthocyanins is derived using the kinetic plot method (KPM). Further, it is shown how analysis under optimal conditions, in combination with MS detection, delivers much improved separation and identification of red wine anthocyanins and their derived products. This improved analytical performance holds promise for the in-depth investigation of these influential compounds in wine during ageing. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

Beyer, W F

1976-12-01

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

Method for the chromatographic separation of cations from aqueous samples

DOEpatents

Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

1997-07-29

An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methanediphosphonic acid on an inert particulate support. 7 figs.

Method for the chromatographic separation of cations from aqueous samples

DOEpatents

Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

1998-12-22

An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methane-diphosphonic acid on an inert particulate support. 7 figs.

Determination of trihalomethanes in waters by ionic liquid-based single drop microextraction/gas chromatographic/mass spectrometry.

PubMed

Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

2008-10-31

A simple, rapid, solventless method for the determination of trihalomethanes (THMs) (chloroform, bromodichloromethane, dibromochloromethane and bromoform) in water samples is presented. The analytes are extracted from the headspace of the aqueous matrix into a 2 microL drop of the ionic liquid 1-octyl-3-methyl-imidazolium hexafluorophosphate working at 30 degrees C for 30 min. The separation and detection of the target compounds is accomplished by gas chromatography/mass spectrometry owing to the use of an interface that efficiently transfers the analytes extracted in the ionic liquid drop to the gas chromatograph while preventing the ionic liquid from entering the column. The detection limits obtained are below the values compelled by the legislation, ranging from 0.5 microg L(-1) for chloroform and bromodichloromethane to 0.9 microg L(-1) for dibromochloromethane. The use of ionic liquid in the extraction procedure avoids the use of organic solvents and leads to relative standard deviations that range from 3.1% to 4.8%.

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

PubMed

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

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

Gas-liquid chromatographic method for determining ethylenethiourea in potatoes, spinach, applesauce, and milk: collaborative study.

PubMed

Onley, H H

1977-09-01

Eight laboratories collaboratively tested a gas-liquid chromatographic method for determining ethylenetiourea (ETU) in potatoes, spinach, applesauce, and milk. In the determinative step, ETU is converted to the S-butyl derivative (2-n-butylmercapto-2-imidazoline) which is detected by a flame photometric detector, sulfur mode. For unknown fortification levels of 0.06, 0.12, and 0.30 ppm, the collaborators reported an overall average recovery range of 85-97% in the various commodities. The method has been adopted as interim official first action.

Liquid fractionation. Part I: Basic principles and experimental simulations

NASA Astrophysics Data System (ADS)

McBirney, Alexander R.; Baker, Brian H.; Nilson, Robert H.

1985-03-01

A possible explanation for the closely associated magmas of contrasting compositions erupted from many mature volcanic centers can be found in the large differences of density produced by relatively small compositional variations in liquids that evolve by crystallization or melting at the walls of shallow magma chambers. A mechanism of liquid fractionation in which differentiated liquids segragate gravitationally to form compositionally graded columns of magma may surmount the long-standing problem of explaining large volumes of highly evolved liquids that reach advanced degrees of differentiation in times that are too short to be consistent with conventional models of crystal fractionation based on crystal settling. In those types of magmas that decrease in density as they differentiate, a fractionated liquid next to a wall may form a buoyant compositional boundary layer that flows up the wall and accumulates as a separate zone in the upper levels of the reservoir. Magmas that increase in density as they differentiate will have the opposite behavior; they descend along the wall and pond on the floor. Both types of systems can be modeled using simple aqueous solutions and techniques similar to those developed by Chen and Turner (1980). The insights gained through experiments of this kind suggest a number of processes that may be responsible for common types of volcanic behavior and patterns of differentiation in shallow plutons.

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

EPA Science Inventory

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

Fractional Consumption of Liquid Hydrogen and Liquid Oxygen During the Space Shuttle Program

NASA Technical Reports Server (NTRS)

Partridge, Jonathan K.

2011-01-01

The Space Shuttle uses the propellants, liquid hydrogen and liquid oxygen, to meet part of the propulsion requirements from ground to orbit. The Kennedy Space Center procured over 25 million kilograms of liquid hydrogen and over 250 million kilograms of liquid oxygen during the 3D-year Space Shuttle Program. Because of the cryogenic nature of the propellants, approximately 55% of the total purchased liquid hydrogen and 30% of the total purchased liquid oxygen were used in the Space Shuttle Main Engines. The balance of the propellants were vaporized during operations for various purposes. This paper dissects the total consumption of liqUid hydrogen and liqUid oxygen and determines the fraction attributable to each of the various processing and launch operations that occurred during the entire Space Shuttle Program at the Kennedy Space Center.

Aging of SRC liquids

NASA Astrophysics Data System (ADS)

Hara, T.; Jones, L.; Tewari, K. C.; Li, N. C.

1981-02-01

The viscosity of SRC-LL liquid increases when subjected to accelerated aging by bubbling oxygen in the presence of copper strip at 62°C. Precipitates are formed and can be separated from the aged liquid by Soxhlet extraction with pentane. A 30-70 blend of SRC-I with SRC-LL was subjected to oxygen aging in the absence of copper, and the viscosity increased dramatically after 6 days at 62°. The content of preasphaltene and its molecular size increase with time of aging, accompanied by decrease of asphaltene and pentane-soluble contents. For the preasphaltene fraction on aging, gel permeation chromatography shows formation of larger particles. ESR experiments show that with oxygen aging, spin concentration in the preasphaltene fraction decreases. Perhaps some semiquinone, together with di- and tri-substituted phenoxy radicals, generated by oxygen aging of the coal liquid, interact with the free radicals already present in coal to yield larger particles and reduce free radical concentration. We are currently using the very high-field (600-MHz) NMR spectrometer at Mellon Institute to determine changes in structural parameters before and after aging of SRC-II and its chromatographically separated fractions.

Two tools for applying chromatographic retention data to the mass-based identification of peptides during hydrogen/deuterium exchange experiments by nano-liquid chromatography/matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Gershon, P D

2010-12-15

Two tools are described for integrating LC elution position with mass-based data in hydrogen-deuterium exchange (HDX) experiments by nano-liquid chromatography/matrix-assisted laser desorption/ionization mass spectrometry (nanoLC/MALDI-MS, a novel approach to HDX-MS). The first of these, 'TOF2H-Z Comparator', highlights peptides in HDX experiments that are potentially misidentified on the basis of mass alone. The program first calculates normalized values for the organic solvent concentration responsible for the elution of ions in nanoLC/MALDI HDX experiments. It then allows the solvent gradients for the multiple experiments contributing to an MS/MS-confirmed peptic peptide library to be brought into mutual alignment by iteratively re-modeling variables among LC parameters such as gradient shape, solvent species, fraction duration and LC dead time. Finally, using the program, high-probability chromatographic outliers can be flagged within HDX experimental data. The role of the second tool, 'TOF2H-XIC Comparator', is to normalize the LC chromatograms corresponding to all deuteration timepoints of all HDX experiments of a project, to a common reference. Accurate normalization facilitates the verification of chromatographic consistency between all ions whose spectral segments contribute to particular deuterium uptake plots. Gradient normalization in this manner revealed chromatographic inconsistencies between ions whose masses were either indistinguishable or separated by precise isotopic increments. Copyright © 2010 John Wiley & Sons, Ltd.

Quantum Spin Liquids and Fractionalization

NASA Astrophysics Data System (ADS)

Misguich, Grégoire

This chapter discusses quantum antiferromagnets which do not break any symmetries at zero temperature - also called "spin liquids" - and focuses on lattice spin models with Heisenberg-like (i.e. SU(2)-symmetric) interactions in dimensions larger than one. We begin by discussing the Lieb-Schultz-Mattis theorem and its recent extension to D > 1 by Hastings (2004), which establishes an important distinction between spin liquids with an integer and with a half-integer spin per unit cell. Spin liquids of the first kind, "band insulators", can often be understood by elementary means, whereas the latter, "Mott insulators", are more complex (featuring "topological order") and support spin-1/2 excitations (spinons). The fermionic formalism (Affleck and Marston, 1988) is described and the effect of fluctuations about mean-field solutions, such as the possible creation of instabilities, is discussed in a qualitative way. In particular, we explain the emergence of gauge modes and their relation to fractionalization. The concept of the projective symmetry group (X.-G. Wen, 2002) is introduced, with the aid of some examples. Finally, we present the phenomenology of (gapped) short-ranged resonating-valence-bond spin liquids, and make contact with the fermionic approach by discussing their description in terms of a fluctuating Z 2 gauge field. Some recent references are given to other types of spin liquid, including gapless ones.

Chromatographic and spectroscopic methods for the determination of solvent properties of room temperature ionic liquids.

PubMed

Poole, Colin F

2004-05-28

Room temperature ionic liquids are novel solvents with favorable environmental and technical features. Synthetic routes to over 200 room temperature ionic liquids are known but for most ionic liquids physicochemical data are generally lacking or incomplete. Chromatographic and spectroscopic methods afford suitable tools for the study of solvation properties under conditions that approximate infinite dilution. Gas-liquid chromatography is suitable for the determination of gas-liquid partition coefficients and activity coefficients as well as thermodynamic constants derived from either of these parameters and their variation with temperature. The solvation parameter model can be used to define the contribution from individual intermolecular interactions to the gas-liquid partition coefficient. Application of chemometric procedures to a large database of system constants for ionic liquids indicates their unique solvent properties: low cohesion for ionic liquids with weakly associated ions compared with non-ionic liquids of similar polarity; greater hydrogen-bond basicity than typical polar non-ionic solvents; and a range of dipolarity/polarizability that encompasses the same range as occupied by the most polar non-ionic liquids. These properties can be crudely related to ion structures but further work is required to develop a comprehensive approach for the design of ionic liquids for specific applications. Data for liquid-liquid partition coefficients is scarce by comparison with gas-liquid partition coefficients. Preliminary studies indicate the possibility of using the solvation parameter model for interpretation of liquid-liquid partition coefficients determined by shake-flask procedures as well as the feasibility of using liquid-liquid chromatography for the convenient and rapid determination of liquid-liquid partition coefficients. Spectroscopic measurements of solvatochromic and fluorescent probe molecules in room temperature ionic liquids provide insights into

[Evaluation of chromatographic performance of polymerized ionic liquid stationary phase for capillary gas chromatography].

PubMed

Chen, Xiaoyan; Lu, Kai; Qi, Meiling; Fu, Ruonong

2009-11-01

The selectivity and thermal stability of ionic liquids as the stationary phases for capillary gas chromatography (CGC) have attracted much attention of researchers in recent years. In this study, 1-vinyl-3-benzyl imidazolium-bis(trifluoromethane-sulphonyl)imidate (VBIm-NTf2) was synthesized and polymerized (PVBIm-NTf2) in a CGC column. In comparison with VBIm-NTf2, PVBIm-NTf2 exhibits much better thermal stability and chromatographic selectivity, and achieves satisfactory resolution for Grob test mixture, alcohols mixture, esters mixture and aromatics mixture with narrow and symmetric peak shapes. The satisfactory resolution and selectivity of the polymerized column still remain after conditioned at 250 degrees C for 6 h. Additionally, the Abraham solvation parameters of PVBIm-NTf2 were determined and the interactions between the stationary phase and solutes were elucidated. The present work demonstrates that the polymerization is an effective way to improve the selectivity and thermal stability of common ionic liquids as CGC stationary phases.

LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF TRANS-CHLORDANE, CIS-CHLORDANE, HEPTACHLOR, HEPTACHLOR EPOXIDE AND ALPHA-HEXACHLOROCYCLOHEXANE WITH APPLICATION TO SMALL-SCALE PREPARATIVE SEPARATION

EPA Science Inventory

Analytical high-performance liquid chromatographic separations of the individual enantiomers of five polychlorinated compounds were obtained on polysaccharide stereoselective HPLC columns. The enantiomers of the pesticides trans-chlordane, cis-chlordane and heptachlor were separa...

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

PubMed

Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

2013-11-01

A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Alternative solvent-based methyl benzoate vortex-assisted dispersive liquid-liquid microextraction for the high-performance liquid chromatographic determination of benzimidazole fungicides in environmental water samples.

PubMed

Santaladchaiyakit, Yanawath; Srijaranai, Supalax

2014-11-01

Vortex-assisted dispersive liquid-liquid microextraction using methyl benzoate as an alternative extraction solvent for extracting and preconcentrating three benzimidazole fungicides (i.e., carbendazim, thiabendazole, and fluberidazole) in environmental water samples before high-performance liquid chromatographic analysis has been developed. The selected microextraction conditions were 250 μL of methyl benzoate containing 300 μL of ethanol, 1.0% w/v sodium acetate, and vortex agitation speed of 2100 rpm for 30 s. Under optimum conditions, preconcentration factors were 14.5-39.0 for the target fungicides. Limits of detection were obtained in the range of 0.01-0.05 μg/L. The proposed method was then applied to surface water samples and the recovery evaluations at three spiked concentration levels of 5, 30, and 50 μg/L were obtained in the range of 77.4-110.9% with the relative standard deviation <7.4%. The present method was simple, rapid, low cost, sensitive, environmentally friendly, and suitable for the trace analysis of the studied fungicides in environmental water samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Real-space imaging of fractional quantum Hall liquids

NASA Astrophysics Data System (ADS)

Hayakawa, Junichiro; Muraki, Koji; Yusa, Go

2013-01-01

Electrons in semiconductors usually behave like a gas--as independent particles. However, when confined to two dimensions under a perpendicular magnetic field at low temperatures, they condense into an incompressible quantum liquid. This phenomenon, known as the fractional quantum Hall (FQH) effect, is a quantum-mechanical manifestation of the macroscopic behaviour of correlated electrons that arises when the Landau-level filling factor is a rational fraction. However, the diverse microscopic interactions responsible for its emergence have been hidden by its universality and macroscopic nature. Here, we report real-space imaging of FQH liquids, achieved with polarization-sensitive scanning optical microscopy using trions (charged excitons) as a local probe for electron spin polarization. When the FQH ground state is spin-polarized, the triplet/singlet intensity map exhibits a spatial pattern that mirrors the intrinsic disorder potential, which is interpreted as a mapping of compressible and incompressible electron liquids. In contrast, when FQH ground states with different spin polarization coexist, domain structures with spontaneous quasi-long-range order emerge, which can be reproduced remarkably well from the disorder patterns using a two-dimensional random-field Ising model. Our results constitute the first reported real-space observation of quantum liquids in a class of broken symmetry state known as the quantum Hall ferromagnet.

Biogas production from the mechanically pretreated, liquid fraction of sorted organic municipal solid wastes.

PubMed

Alvarado-Lassman, A; Méndez-Contreras, J M; Martínez-Sibaja, A; Rosas-Mendoza, E S; Vallejo-Cantú, N A

2017-06-01

The high liquid content in fruit and vegetable wastes makes it convenient to mechanically separate these wastes into mostly liquid and solid fractions by means of pretreatment. Then, the liquid fraction can be treated using a high-rate anaerobic biofilm reactor to produce biogas, simultaneously reducing the amount of solids that must be landfilled. In this work, the specific composition of municipal solid waste (MSW) in a public market was determined; then, the sorted organic fraction of municipal solid waste was treated mechanically to separate and characterize the mostly liquid and solid fractions. Then, the mesophilic anaerobic digestion for biogas production of the first fraction was evaluated. The anaerobic digestion resulted in a reduced hydraulic retention time of two days with high removal of chemical oxygen demand, that is, 88% on average, with the additional benefit of reducing the mass of the solids that had to be landfilled by about 80%.

Experimental evidence for Mo isotope fractionation between metal and silicate liquids

NASA Astrophysics Data System (ADS)

Hin, Remco C.; Burkhardt, Christoph; Schmidt, Max W.; Bourdon, Bernard; Kleine, Thorsten

2013-10-01

Stable isotope fractionation of siderophile elements may inform on the conditions and chemical consequences of core-mantle differentiation in planetary objects. The extent to which Mo isotopes fractionate during such metal-silicate segregation, however, is so far unexplored. We have therefore investigated equilibrium fractionation of Mo isotopes between liquid metal and liquid silicate to evaluate the potential of Mo isotopes as a new tool to study core formation. We have performed experiments at 1400 and 1600 °C in a centrifuging piston cylinder. Tin was used to lower the melting temperature of the Fe-based metal alloys to <1400 °C, while variable Fe-oxide contents were used to vary oxygen fugacity in graphite and MgO capsules. Isotopic analyses were performed using a double spike technique. In experiments performed at 1400 °C, the 98Mo/95Mo ratio of silicate is 0.19±0.03‰ (95% confidence interval) heavier than that of metal. This fractionation is not significantly affected by the presence or absence of carbon. Molybdenum isotope fractionation is furthermore independent of oxygen fugacity in the range IW -1.79 to IW +0.47, which are plausible values for core formation. Experiments at 1600 °C show that, at equilibrium, the 98Mo/95Mo ratio of silicate is 0.12±0.02‰ heavier than that of metal and that the presence or absence of Sn does not affect this fractionation. Equilibrium Mo isotope fractionation between liquid metal and liquid silicate as a function of temperature can therefore be described as ΔMoMetal-Silicate98/95=-4.70(±0.59)×105/T2. Our experiments show that Mo isotope fractionation may be resolvable up to metal-silicate equilibration temperatures of about 2500 °C, rendering Mo isotopes a novel tool to investigate the conditions of core formation in objects ranging from planetesimals to Earth sized bodies.

Separation of the fatty acids in menhaden oil as methyl esters with a highly polar ionic liquid gas chromatographic column and identification by time of flight mass spectrometry.

PubMed

Fardin-Kia, Ali Reza; Delmonte, Pierluigi; Kramer, John K G; Jahreis, Gerhard; Kuhnt, Katrin; Santercole, Viviana; Rader, Jeanne I

2013-12-01

The fatty acids contained in marine oils or products are traditionally analyzed by gas chromatography using capillary columns coated with polyethylene glycol phases. Recent reports indicate that 100 % cyanopropyl siloxane phases should also be used when the analyzed samples contain trans fatty acids. We investigated the separation of the fatty acid methyl esters prepared from menhaden oil using the more polar SLB-IL111 (200 m × 0.25 mm) ionic liquid capillary column and the chromatographic conditions previously optimized for the separation of the complex mixture of fatty acid methyl esters prepared from milk fat. Identifications of fatty acids were achieved by applying Ag(+)-HPLC fractionation and GC-TOF/MS analysis in CI(+) mode with isobutane as the ionization reagent. Calculation of equivalent chain lengths confirmed the assignment of double bond positions. This methodology allowed the identification of 125 fatty acids in menhaden oil, including isoprenoid and furanoid fatty acids, and the novel 7-methyl-6-hexadecenoic and 7-methyl-6-octadecenoic fatty acids. The chromatographic conditions applied in this study showed the potential of separating in a single 90-min analysis, among others, the short chain and trans fatty acids contained in dairy products, and the polyunsaturated fatty acids contained in marine products.

Recycling the liquid fraction of alkaline hydrogen peroxide in the pretreatment of corn stover.

PubMed

Alencar, Bárbara Ribeiro Alves; Reis, Alexandre Libanio Silva; de Souza, Raquel de Fatima Rodrigues; Morais, Marcos Antônio; Menezes, Rômulo Simões Cezar; Dutra, Emmanuel Damilano

2017-10-01

The aim of this study was to evaluate the influence of recycling the liquid fraction of pretreatment with alkaline hydrogen peroxide (AHP) on the hydrolysis of corn stover. Corn stover was pretreated in the traditional condition with 7.5% v/v H 2 O 2 . After pretreatment, the solids were separated from the liquid fraction and five successive reuse cycles of the liquid fraction were tested. The solid fraction from pretreatment in each recycle was submitted to enzymatic hydrolysis. The number of recycles had a linear negative effect (R 2 =0.98) on biomass delignification efficiency and also affected negatively the enzymatic conversion efficiency. Despite the decrease in efficiency after each recycling step, reuse of the liquid fraction leads to reduction in water, H 2 O 2 and NaOH consumption of up to 57.6%, 59.6% and 57.6%, respectively. These findings point to an efficient recycling technology, which may reduce costs and save water. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

PubMed

Gartzke, J; Jäger, H; Vins, I

1991-01-01

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

Comparison of rumen bacteria distribution in original rumen digesta, rumen liquid and solid fractions in lactating Holstein cows.

PubMed

Ji, Shoukun; Zhang, Hongtao; Yan, Hui; Azarfar, Arash; Shi, Haitao; Alugongo, Gibson; Li, Shengli; Cao, Zhijun; Wang, Yajing

2017-01-01

Original rumen digesta, rumen liquid and solid fractions have been frequently used to assess the rumen bacterial community. However, bacterial profiles in rumen original digesta, liquid and solid fractions vary from each other and need to be better established. To compare bacterial profiles in each fraction, samples of rumen digesta from six cows fed either a high fiber diet (HFD) or a high energy diet (HED) were collected via rumen fistulas. Rumen digesta was then squeezed through four layers of cheesecloth to separate liquid and solid fractions. The bacterial profiles of rumen original digesta, liquid and solid fractions were analyzed with High-throughput sequencing technique. Rumen bacterial diversity was mainly affected by diet and individual cow ( P  > 0.05) rather than rumen fraction. Bias distributed bacteria were observed in solid and liquid fractions of rumen content using Venn diagram and LEfSe analysis. Fifteen out of 16 detected biomarkers (using LEfSe analysis) were found in liquid fraction, and these 15 biomarkers contributed the most to the bacterial differences among rumen content fractions. Similar results were found when using samples of original rumen digesta, rumen liquid or solid fractions to assess diversity of rumen bacteria; however, more attention should be draw onto bias distributed bacteria in different ruminal fractions, especially when liquid fraction has been used as a representative sample for rumen bacterial study.

A Versatile, Automatic Chromatographic Column Packing Device

ERIC Educational Resources Information Center

Barry, Eugene F.; And Others

1977-01-01

Describes an inexpensive apparatus for packing liquid and gas chromatographic columns of high efficiency. Consists of stainless steel support struts, an Automat Getriebmotor, and an associated three-pulley system capable of 10, 30, and 300 rpm. (MLH)

A versatile liquid chromatographic technique for pharmacokinetic estimation of curcumin in human plasma.

PubMed

Gugulothu, Dalapathi; Desai, Preshita; Patravale, Vandana

2014-09-01

A simple, rapid, sensitive and specific liquid chromatographic method was developed and validated for the determination of curcumin in human plasma. Berberine was used as the internal standard. Chromatographic separation was achieved on a Zorbax Eclipse C18 column at 40 °C, with a mobile phase consisting of 1% acetic acid (pH 3 adjusted with 50% triethanolamine): acetonitrile (55:45), at a flow rate of 1.25 mL/min. The method was validated for precision, accuracy, linearity, lower limit of quantification (LLOQ) and extraction efficiency according to the International Conference on Harmonization guidelines. The method was successfully developed with an LLOQ of 10 ng/mL and a runtime of 9 min. Linearity range was from 10 to 1000 ng/mL. Curcumin and Berberine were well separated with retention times of 8.2 ± 0.2 and 1.4 ± 0.1 min, respectively. Further, the method was successfully employed to study the pharmacokinetic parameters of curcumin, following oral administration of curcumin-loaded hydroxy propyl cellulose (HPC) nanoparticles and curcumin suspension in female Wistar rats. Curcumin-loaded HPC nanoparticles (Cmax: 106.01 ± 20.11 ng/mL) showed significant improvement in pharmacokinetic parameters when compared with curcumin suspension (Cmax: 30.13 ± 0.47 ng/mL) indicating 43.73-fold increase in relative bioavailability. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Simple, fast and reliable liquid chromatographic and spectrophotometric methods for the determination of theophylline in urine, saliva and plasma samples.

PubMed

Charehsaz, Mohammad; Gürbay, Aylin; Aydin, Ahmet; Sahin, Gönül

2014-01-01

In this study, a high-performance liquid chromatographic method (HPLC) and UV spectrophotometric method were developed, validated and applied for the determination of theophylline in biological fluids. Liquid- liquid extraction is performed for isolation of the drug and elimination of plasma and saliva interferences. Urine samples were applied without any extraction. The chromatographic separation was achieved on a C18 column by using 60:40 methanol:water as mobile phase under isocratic conditions at a flow rate of 0.75 mL/min with UV detection at 280 nm in HPLC method. UV spectrophotometric analysis was performed at 275 nm. the limit of quantification: 1.1 µg/mL for urine, 1.9 µg/mL for saliva, 3.1 µg/mL for plasma; recovery: 94.85% for plasma, 100.45% for saliva, 101.39% for urine; intra-day precision: 0.22-2.33%, inter-day precision: 3.17-13.12%. Spectrophotometric analysis results were as follows: the limit of quantitation: 5.23 µg/mL for plasma, 8.7 µg/mL for urine; recovery: 98.27% for plasma, 95.25% for urine; intra-day precision: 2.37 - 3.00%, inter-day precision: 5.43-7.91%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of theophylline in biological samples. Also spectrophotometric analysis can be used where it can be applicable.

Performance of chromatographic systems to model soil-water sorption.

PubMed

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

2012-08-24

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

Quantitative Metabolome Analysis Based on Chromatographic Peak Reconstruction in Chemical Isotope Labeling Liquid Chromatography Mass Spectrometry.

PubMed

Huan, Tao; Li, Liang

2015-07-21

Generating precise and accurate quantitative information on metabolomic changes in comparative samples is important for metabolomics research where technical variations in the metabolomic data should be minimized in order to reveal biological changes. We report a method and software program, IsoMS-Quant, for extracting quantitative information from a metabolomic data set generated by chemical isotope labeling (CIL) liquid chromatography mass spectrometry (LC-MS). Unlike previous work of relying on mass spectral peak ratio of the highest intensity peak pair to measure relative quantity difference of a differentially labeled metabolite, this new program reconstructs the chromatographic peaks of the light- and heavy-labeled metabolite pair and then calculates the ratio of their peak areas to represent the relative concentration difference in two comparative samples. Using chromatographic peaks to perform relative quantification is shown to be more precise and accurate. IsoMS-Quant is integrated with IsoMS for picking peak pairs and Zero-fill for retrieving missing peak pairs in the initial peak pairs table generated by IsoMS to form a complete tool for processing CIL LC-MS data. This program can be freely downloaded from the www.MyCompoundID.org web site for noncommercial use.

Liquid chromatographic determination of histamine in fish, sauerkraut, and wine: interlaboratory study.

PubMed

Beljaars, P R; Van Dijk, R; Jonker, K M; Schout, L J

1998-01-01

An interlaboratory study of the liquid chromatographic (LC) determination of histamine in fish, sauerkraut, and wine was conducted. Diminuted and homogenized samples were suspended in water followed by clarification of extracts with perchloric acid, filtration, and dilution with water. After LC separation on a reversed-phase C18 column with phosphate buffer (pH 3.0)--acetonitrile (875 + 125, v/v) as mobile phase, histamine was measured fluorometrically (excitation, 340 nm; emission, 455 nm) in samples and standards after postcolumn derivatization with o-phthaldialdehyde (OPA). Fourteen samples (including 6 blind duplicates and 1 split level) containing histamine at about 10-400 mg/kg or mg/L were analyzed singly according to the proposed procedure by 11 laboratories. Results from one participant were excluded from statistical analysis. For all samples analyzed, repeatability relative standard deviations varied from 2.1 to 5.6%, and reproducibility relative standard deviations ranged from 2.2 to 7.1%. Averaged recoveries of histamine for this concentration range varied from 94 to 100%.

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

PubMed

Spurlock, C H; Schneider, H G

1984-01-01

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

Characterization of a chemical artifact in the liquid chromatographic determination of 3-butyn-2-one using the 2,4-dinitrophenylhydrazine method.

PubMed

Vogel, M; Pötter, W; Karst, U

2000-07-21

This study reports the identification of a chemical artifact occurring in the liquid chromatographic analysis of 3-butyn-2-one by means of the 2,4-dinitrophenylhydrazine (DNPH) method. Besides the expected derivatization reaction to the corresponding butynone DNPhydrazone, a rearrangement was observed, thus leading to the formation of 3-methyl-1-(2',4'-dinitrophenyl)pyrazol (DNPP). Although the rearrangement product and the hydrazone can easily be separated by means of liquid chromatography, problems arise from coelution of the pyrazol with the formaldehyde DNPhydrazone. Identification of the artifact by means of UV-Vis spectroscopy using dual wavelength or diode array detection is discussed.

Gas-liquid chromatography with a volatile "stationary" liquid phase.

PubMed

Wells, P S; Zhou, S; Parcher, J F

2002-05-01

A unique type of gas-liquid chromatography is described in which both mobile and "stationary" phases are composed of synthetic mixtures of helium and carbon dioxide. At temperatures below the critical point of the binary mixture and pressures above the vapor pressure of pure liquid carbon dioxide, helium and carbon dioxide can form two immiscible phases over extended composition ranges. A binary vapor phase enriched in helium can act as the mobile phase for chromatographic separations, whereas a CO2-rich liquid in equilibrium with the vapor phase, but condensed on the column wall, can act as a pseudostationary phase. Several examples of chromatographic separations obtained in "empty" capillary columns with no ordinary stationary liquid phase illustrate the range of conditions that produce such separations. In addition, several experiments are reported that confirm the proposed two-phase hypothesis. The possible consequences of the observed chromatographic phenomenon in the field of supercritical fluid chromatography with helium headspace carbon dioxide are discussed.

Estimation of liquid volume fraction using ultrasound transit time spectroscopy

NASA Astrophysics Data System (ADS)

Al-Qahtani, Saeed M.; Langton, Christian M.

2016-12-01

It has recently been proposed that the propagation of an ultrasound wave through complex structures, consisting of two-materials of differing ultrasound velocity, may be considered as an array of parallel ‘sonic rays’, the transit time of each determined by their relative proportion; being a minimum (t min) in entire higher velocity material, and a maximum (t max) in entire lower velocity material. An ultrasound transit time spectrum (UTTS) describes the proportion of sonic rays at an individual transit time. It has previously been demonstrated that the solid volume fraction of a solid:liquid composite, specifically acrylic step-wedges immersed in water, may be reliably estimated from the UTTS. The aim of this research was to investigate the hypothesis that the volume fraction of a two-component liquid mixture, of unequal ultrasound velocity, may also be estimated by UTTS. A through-transmission technique incorporating two 1 MHz ultrasound transducers within a horizontally-aligned cylindrical tube-housing was utilised, the proportion of silicone oil to water being varied from 0% to 100%. The liquid volume fraction was estimated from the UTTS at each composition, the coefficient of determination (R 2%) being 98.9  ±  0.7%. The analysis incorporated a novel signal amplitude normalisation technique to compensate for absorption within the silicone oil. It is therefore envisaged that the parallel sonic ray concept and the derived UTTS may be further applied to the quantification of liquid mixture composition assessment.

Liquid chromatographic determination of benzocaine and N-acetylbenzocaine in the edible fillet tissue from rainbow trout

USGS Publications Warehouse

Meinertz, J.R.; Stehly, G.R.; Hubert, T.D.; Bernardy, J.A.

1999-01-01

A method was developed for determining benzocaine and N-acetylbenzocaine concentrations in fillet tissue of rainbow trout. The method involves extracting the analytes with acetonitrile, removing lipids or hydrophobic compounds from the extract with hexane, and providing additional clean-up with solid-phase extraction techniques. Analyte concentrations are determined using reversed-phase high-performance liquid chromatographic techniques with an isocratic mobile phase and UV detection. The accuracy (range, 92 to 121%), precision (R.S.D., <14%), and sensitivity (method quantitation limit, <24 ng/g) for each analyte indicate the usefulness of this method for studies characterizing the depletion of benzocaine residues from fish exposed to benzocaine. Copyright (C) 1999.

Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

PubMed

Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

2016-06-01

In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance liquid chromatographic determination of benzil in air as an indicator of emissions derived from polyester powder coatings.

PubMed

Pukkila, J; Kokotti, H; Peltonen, K

1989-10-06

A method to estimate occupational exposure to emissions from the curing of polyester powder paints was developed. The method is based on the monitoring only of a certain marker compound in workroom air in order to make the determinations easier. Benzil, reproducibly emitted from all the powders tested, was chosen as the indicator for curing (220 degrees C)-derived emissions. A method for the air sampling and high-performance liquid chromatographic benzil is described. Aspects of the use of marker compounds are discussed.

High-pressure liquid chromatography of aromatic amines

NASA Technical Reports Server (NTRS)

Young, P. R.

1979-01-01

Analysis made on commercially available liquid chromatograph demonstrates high-pressure liquid chromatographic conditions for separation of approximately 50 aromatic amines ranging from simple aniline derivatives to complex multiring di- and tri-amines.

Effect of hawthorn (Crataegus oxycantha) crude extract and chromatographic fractions on multiple activities in a cultured cardiomyocyte assay.

PubMed

Long, S R; Carey, R A; Crofoot, K M; Proteau, P J; Filtz, T M

2006-11-01

Extracts of hawthorn (Crataegus oxycantha) have become popular herbal supplements for their well-recognized cardiotonic effects. Many commercial preparations have been used successfully in the treatment of congestive heart failure, although the active principles within these extracts have yet to be conclusively identified. Several hawthorn preparations were studied and found to have negative chronotropic effects in a cultured neonatal murine cardiomyocyte assay using unpaced cells. As compared to conventional cardiac drugs (i.e., epinephrine, milrinone, ouabain, or propranolol), hawthorn extract has a unique activity profile. Hawthorn extract appears to be anti-arrhythmic and capable of inducing rhythmicity in quiescent cardiomyocytes. Hawthorn extract does not cause beta-adrenergic receptor blockade at concentrations which cause negative chronotropic effects. Commercial hawthorn preparations, extracts prepared from dried leaves and those made from dried berries have similar chronotropic activities. When crude extracts are separated using size-exclusion chromatography, several fractions retain multiple cardiac activities. Assays with chromatographic fractions reveal that multiple dissimilar cardioactive components may exist within the extract, making the identification of individual active constituents more challenging.

Gas-liquid Phase Distribution and Void Fraction Measurements Using the MRI

NASA Technical Reports Server (NTRS)

Daidzic, N. E.; Schmidt, E.; Hasan, M. M.; Altobelli, S.

2004-01-01

We used a permanent-magnet MRI system to estimate the integral and spatially- and/or temporally-resolved void-fraction distributions and flow patterns in gas-liquid two-phase flows. Air was introduced at the bottom of the stagnant liquid column using an accurate and programmable syringe pump. Air flow rates were varied between 1 and 200 ml/min. The cylindrical non-conducting test tube in which two-phase flow was measured was placed in a 2.67 kGauss MRI with MRT spectrometer/imager. Roughly linear relationship has been obtained for the integral void-fraction, obtained by volume-averaging of the spatially-resolved signals, and the air flow rate in upward direction. The time-averaged spatially-resolved void fraction has also been obtained for the quasi-steady flow of air in a stagnant liquid column. No great accuracy is claimed as this was an exploratory proof-of-concept type of experiment. Preliminary results show that MRI a non-invasive and non-intrusive experimental technique can indeed provide a wealth of different qualitative and quantitative data and is especially well suited for averaged transport processes in adiabatic and diabatic multi-phase and/or multi-component flows.

Optimisation of chromatographic resolution using objective functions including both time and spectral information.

PubMed

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

2015-01-16

The optimisation of the resolution in high-performance liquid chromatography is traditionally performed attending only to the time information. However, even in the optimal conditions, some peak pairs may remain unresolved. Such incomplete resolution can be still accomplished by deconvolution, which can be carried out with more guarantees of success by including spectral information. In this work, two-way chromatographic objective functions (COFs) that incorporate both time and spectral information were tested, based on the peak purity (analyte peak fraction free of overlapping) and the multivariate selectivity (figure of merit derived from the net analyte signal) concepts. These COFs are sensitive to situations where the components that coelute in a mixture show some spectral differences. Therefore, they are useful to find out experimental conditions where the spectrochromatograms can be recovered by deconvolution. Two-way multivariate selectivity yielded the best performance and was applied to the separation using diode-array detection of a mixture of 25 phenolic compounds, which remained unresolved in the chromatographic order using linear and multi-linear gradients of acetonitrile-water. Peak deconvolution was carried out using the combination of orthogonal projection approach and alternating least squares. Copyright © 2014 Elsevier B.V. All rights reserved.

Liquid chromatographic determination of acriflavine and proflavine residues in channel catfish muscle.

PubMed

Plakas, S M; el Said, K R; Jester, E L; Bencsath, F A; Hayton, W L

1997-01-01

A liquid chromatographic (LC) method was developed for determination of acriflavine (ACR) and proflavine (PRO) residues in channel catfish muscle. Residues were extracted with acidified methanol solution, and extracts were cleaned up with C18 solid-phase extraction columns. Residue concentrations were determined on an LC cyano column, with spectrophotometric detection at 454 nm. Catfish muscle was individually fortified with ACR (purified from commercial product) and PRO at concentrations of 5, 10, 20, 40, and 80 ppb (5 replicates per level). Mean recoveries from fortified muscle at each level ranged from 86 to 95%, with relative standard deviations (RSDs) of 2.5 to 5.7%. The method was applied to incurred residues of ACR and PRO in muscle after waterborne exposure of channel catfish to commercial acriflavine (10 ppm total dye for 4 h). RSDs for incurred residues of ACR and PRO were in the same range as those for fortified muscle. Low residue concentrations (< 1% of exposure water concentration) suggested poor absorption of ACR and PRO in catfish.

Liquid Crystals in Chromatography

NASA Astrophysics Data System (ADS)

Witkiewicz, Zygfryd

The following sections are included: * INTRODUCTION * LIQUID CRYSTALS SUITABLE FOR GAS CHROMATOGRAPHY * Monomeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Conventional Analytical Columns * Capillary Columns * FACTORS AFFECTING THE CHROMATOGRAPHIC SEPARATIONS ON LIQUID CRYSTAL STATIONARY PHASES * Kind of Mesophase of the Liquid Crystal * Molecular Structure of the Liquid Crystals and of the Chromatographed Substances * Substrate on which the Liquid Crystal is Deposited * ANALYTICAL APPLICATIONS OF LIQUID CRYSTAL STATIONARY PHASES IN GAS CHROMATOGRAPHY * Separation of Isomers of Benzene and Naphthalene Derivatives * Separation of Alkane and Alkene Isomers * Separation of Mixtures of Benzene and Aliphatic Hydrocarbon Derivatives Containing Heteroatoms * Separation of Polynuclear Hydrocarbons * INVESTIGATION OF THE PROPERTIES OF LIQUID CRYSTALS BY GAS CHROMATOGRAPHY * APPLICATION OF LIQUID CRYSTALS IN LIQUID CHROMATOGRAPHY * Column Chromatography * Thin-Layer Chromatography * APPLICATION OF LIQUID CRYSTAL STATIONARY PHASES IN SUPERCRITICAL FLUID CHROMATOGRAPHY * FINAL REMARKS * References

Concentration and fractionation of hydrophobic organic acid constituents from natural waters by liquid chromatography

USGS Publications Warehouse

Thurman, E.M.; Malcolm, R.L.

1979-01-01

A scheme is presented which used adsorption chromatography with pH gradient elution and size-exclusion chromatography to concentrate and separate hydrophobic organic acids from water. A review of chromatographic processes involved in the flow scheme is also presented. Organic analytes which appear in each aqueous fraction are quantified by dissolved organic carbon analysis. Hydrophobic organic acids in a water sample are concentrated on a porous acrylic resin. These acids usually constitute approximately 30-50 percent of the dissolved organic carbon in an unpolluted water sample and are eluted with an aqueous eluent (dilute base). The concentrate is then passed through a column of polyacryloylmorpholine gel, which separates the acids into high- and low-molecular-weight fractions. The high- and low-molecular-weight eluates are reconcentrated by adsorption chromatography, then are eluted with a pH gradient into strong acids (predominately carboxylic acids) and weak acids (predominately phenolic compounds). For standard compounds and samples of unpolluted waters, the scheme fractionates humic substances into strong and weak acid fractions that are separated from the low molecular weight acids. A new method utilizing conductivity is also presented to estimate the acidic components in the methanol fraction.

Application of ionic liquids in liquid chromatography and electrodriven separation.

PubMed

Huang, Yi; Yao, Shun; Song, Hang

2013-08-01

Ionic liquids (ILs) are salts in the liquid state at ambient temperature, which are nonvolatile, nonflammable with high thermal stability and dissolve easily for a wide range of inorganic and organic materials. As a kind of potential green solvent, they show high efficiency and selectivity in the field of separation research, especially in instrumental analysis. Thus far, ILs have been successfully applied by many related researchers in high-performance liquid chromatography and capillary electrophoresis as chromatographic stationary phases, mobile phase additives or electroosmotic flow modifiers. This paper provides a detailed review of these applications in the study of natural products, foods, drugs and other fine chemicals. Furthermore, the prospects of ILs in liquid chromatographic and electrodriven techniques are discussed.

Fluorescent high-performance liquid chromatographic analysis of vigabatrin enantiomers after derivatizing with naproxen acyl chloride.

PubMed

Hsieh, Chun-Yu; Wang, Shing-Yaw; Kwan, Aij-Lie; Wu, Hsin-Lung

2008-01-18

Vigabatrin is widely used as an anticonvulsant in the treatment of seizures. Vigabatrin is usually supplied as racemate in formulation, but only the (S)-(+)-enantiomer of vigabatrin is pharmacologically active. A simple and sensitive liquid chromatographic method is described for the separation and quantification of vigabatrin enantiomers. The method is based on derivatizing racemic vigabatrin with a fluorescent chiral reagent (naproxen acyl chloride). The resulting diastereomeric derivatives are highly responsive to a fluorimetric detector (lambda(ex)=230 nm, lambda(em)=350 nm). The lower quantitation limit of the method is attainable at 25 nM for (S)-(+)-vigabatrin or (R)-(-)-vigabatrin with a detection limit of about 2.5 nM (S/N=3 with 10 microl injected). Application of the method to the analysis of vigabatrin in serum of dosed patients proved feasible.

Determination of solute descriptors by chromatographic methods.

PubMed

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

2009-10-12

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

Multivariate curve resolution based chromatographic peak alignment combined with parallel factor analysis to exploit second-order advantage in complex chromatographic measurements.

PubMed

Parastar, Hadi; Akvan, Nadia

2014-03-13

In the present contribution, a new combination of multivariate curve resolution-correlation optimized warping (MCR-COW) with trilinear parallel factor analysis (PARAFAC) is developed to exploit second-order advantage in complex chromatographic measurements. In MCR-COW, the complexity of the chromatographic data is reduced by arranging the data in a column-wise augmented matrix, analyzing using MCR bilinear model and aligning the resolved elution profiles using COW in a component-wise manner. The aligned chromatographic data is then decomposed using trilinear model of PARAFAC in order to exploit pure chromatographic and spectroscopic information. The performance of this strategy is evaluated using simulated and real high-performance liquid chromatography-diode array detection (HPLC-DAD) datasets. The obtained results showed that the MCR-COW can efficiently correct elution time shifts of target compounds that are completely overlapped by coeluted interferences in complex chromatographic data. In addition, the PARAFAC analysis of aligned chromatographic data has the advantage of unique decomposition of overlapped chromatographic peaks to identify and quantify the target compounds in the presence of interferences. Finally, to confirm the reliability of the proposed strategy, the performance of the MCR-COW-PARAFAC is compared with the frequently used methods of PARAFAC, COW-PARAFAC, multivariate curve resolution-alternating least squares (MCR-ALS), and MCR-COW-MCR. In general, in most of the cases the MCR-COW-PARAFAC showed an improvement in terms of lack of fit (LOF), relative error (RE) and spectral correlation coefficients in comparison to the PARAFAC, COW-PARAFAC, MCR-ALS and MCR-COW-MCR results. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of Analytical Quality by Design concept for bilastine and its degradation impurities determination by hydrophilic interaction liquid chromatographic method.

PubMed

Terzić, Jelena; Popović, Igor; Stajić, Ana; Tumpa, Anja; Jančić-Stojanović, Biljana

2016-06-05

This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2008-05-23

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

Correlations between chromatographic parameters and bioactivity predictors of potential herbicides.

PubMed

Janicka, Małgorzata

2014-08-01

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

Chromatographic analysis of lipid fractions in healthy dogs and dogs with obesity or hyperadrenocorticism.

PubMed

Jericó, Márcia Marques; De Camargo Chiquito, Fernanda; Kajihara, Kazuo; Moreira, Márcio Antonio Bastistela; Gonzales, Rodrigo; Machado, Fabricio Lorenzini Aranha; Nunes, Valéria Sutti; Catanozi, Sergio; Nakandakare, Edna Regina

2009-03-01

Obesity and endogenous hyperadrenocorticism (HAC) are common clinical conditions in veterinary practice, and both conditions have clinical and laboratory similarities, such as weight gain and dyslipidemia. The objective of the present study was to characterize and compare the lipid profiles and plasma lipoprotein fractions in healthy dogs (n = 10), in obese dogs (n = 10), and in dogs with HAC (n = 6). All of the dogs were client owned. The lipoproteins were separated by fast protein liquid chromatography, and the plasma concentrations of total cholesterol and total triacylglycerol (TAG) were determined by enzymatic methods. When compared with the healthy and obese groups, dogs with HAC had a significant increase (P < 0.01) in the total concentrations of TAGs and cholesterol (CHOL), with higher distribution in the very low-density lipoprotein (VLDL)-CHOL fractions. In addition, the distributions of the high-density lipoprotein (HDL)-CHOL and HDL-TAG fractions were significantly lower (P < 0.01) in dogs with HAC than in healthy dogs. Considering the animals in this study, it was determined that the dogs with HAC differed significantly from the healthy and obese dogs regarding the metabolism of CHOL and TAG, as well as their VLDL and HDL fractions. Similar laboratory findings could allow veterinarians to distinguish obese dogs from those with HAC. In addition, dogs with HAC may be at higher risk for developing metabolic and atherosclerotic complications.

Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

PubMed

Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

1986-07-01

This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

High-performance liquid chromatographic separation of human haemoglobins. Simultaneous quantitation of foetal and glycated haemoglobins.

PubMed

Bisse, E; Wieland, H

1988-12-29

A high-performance liquid chromatographic system, which uses a weak cation exchanger (PolyCATA) together with Bis-Tris buffer (pH 6.47-7.0) and sodium acetate gradients, is described. Samples from adults and newborns were analysed and a clean separation of many minor and major normal and abnormal haemoglobin (Hb) variants was greatly improved. The method allows the separation of minor foetal haemoglobin (HbF) variants and the simultaneous quantitation of HbF and glycated HbA. HbF values correlated well with those obtained by the alkali denaturation method (r = 0.997). The glycated haemoglobin (HbAIc) levels measured in patients with high HbF concentrations correlated with the total glycated haemoglobin determined by bioaffinity chromatography (r = 0.973). The procedure is useful for diagnostic applications and affords an effective and sensitive way of examining blood samples for haemoglobin abnormalities.

Mid-infrared laser-absorption diagnostic for vapor-phase fuel mole fraction and liquid fuel film thickness

NASA Astrophysics Data System (ADS)

Porter, J. M.; Jeffries, J. B.; Hanson, R. K.

2011-02-01

A novel two-wavelength mid-infrared laser-absorption diagnostic has been developed for simultaneous measurements of vapor-phase fuel mole fraction and liquid fuel film thickness. The diagnostic was demonstrated for time-resolved measurements of n-dodecane liquid films in the absence and presence of n-decane vapor at 25°C and 1 atm. Laser wavelengths were selected from FTIR measurements of the C-H stretching band of vapor n-decane and liquid n-dodecane near 3.4 μm (3000 cm-1). n-Dodecane film thicknesses <20 μm were accurately measured in the absence of vapor, and simultaneous measurements of n-dodecane liquid film thickness and n-decane vapor mole fraction (300 ppm) were measured with <10% uncertainty for film thicknesses <10 μm. A potential application of the measurement technique is to provide accurate values of vapor mole fraction in combustion environments where strong absorption by liquid fuel or oil films on windows make conventional direct absorption measurements of the gas problematic.

Liquid chromatographic determination of minocycline in brain-to-plasma distribution studies in the rat.

PubMed

Colovic, Milena; Caccia, Silvio

2003-07-05

An isocratic reversed-phase high-performance liquid chromatographic procedure was developed for the determination of minocycline in rat plasma and brain and applied to brain-to-blood (plasma) distribution studies. The procedure is based on isolation of the compound and the internal standard (either demeclocycline or tetracycline may be used) from plasma and brain constituents using the Oasis HLB cartridge, with satisfactory recovery and specificity, and separation on a Symmetry Shield RP8 (15 cm x 4.6 mm, 3.5 microm) column coupled with a UV detector set at 350 nm. The assay was linear over a wide range, with a lower limit of quantification of 50 ng ml(-1) or g(-1), using 0.2 ml of plasma and about 200 mg of brain tissue. Precision and accuracy were acceptable. In the rat minocycline crossed the blood-brain barrier slowly, achieving mean brain concentrations between 30 and 40% of the equivalent systemic exposure, regardless of the dose and route of administration.

Liquid chromatographic determination of urinary 5-methyl-2'-deoxycytidine and pseudouridine as potential biological markers for leukaemia.

PubMed

Zambonin, C G; Aresta, A; Palmisano, F; Specchia, G; Liso, V

1999-12-01

A simple reversed-phase liquid chromatographic (LC) method for the determination of urinary 5-methyl-2'-deoxycytidine (m5dCyd), recently claimed (on the basis of an imuno-technique) to be a potential marker for leukaemia, has been developed. Sample pre-treatment is based on a microcolumn clean-up step with an average recovery of 79% and a RSD of 3%. Detection limit was 0.2 microg/ml which is about tenfold lower than levels previously measured by an ELISA method in urine of healthy individuals. The creatinine (Cre) excretion, necessary for normalising the m5dCyd excretion, was evaluated by ion-pair liquid chromatography which permitted the simultaneous determination of pseudouridine (psi), a modified nucleoside also potentially useful as a marker for leukaemia. The described LC procedures were applied to the analysis of urine samples from healthy individuals and leukaemia patients. While the urinary psi/Cre ratio was found significantly increased for leukaemia patients, the urinary m5dCyd levels in healthy individuals were below the detection limits and did not increase in presence of the malignant disease.

A validated high performance liquid chromatograph-photodiode array method for simultaneous determination of 10 bioactive components in compound hongdoushan capsule

PubMed Central

Zhu, Liancai; Yang, Xian; Tan, Jun; Wang, Bochu; Zhang, Xue

2014-01-01

Background: The compound Hongdoushan capsule (CHC) is widely known as compound herbal preparation and is often used to treat ovarian cancer and breast cancer, and to enhance the body immunity, etc., in clinical practice. Objective: To determine simultaneously 10 bioactive components from CHC, namely glycyrrhetinic acid, liquiritin, glycyrrhizin, baccatin III, 10-deacetylbaccatin III, cephalomannine, taxol, ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1. Materials and Methods: A high performance liquid chromatograph method coupled with photodiode array detector was developed and validated for the 1st time. Chromatographic analysis was performed on a SHIMADZU C18 by utilizing a gradient elution program. The mobile phase was acetonitrile (A)-water (B) at a flow rate of 0.8 mL/min. Results: The calibration curve was linear over the investigated concentration ranges with the values of r2 higher than 0.9993 for all the 10 bioactive components. The average recovery rates range from 98.4% to 100.5% with relative standard deviations ≤2.9%. The developed method was successfully applied to analyze 10 compounds in six CHC samples from different batches. In addition, the herbal sources of 32 chromatographic peaks were identified through comparative studying on chromatograms of standard, the respective extracts of Hongdoushan, RenShen, GanCao, and CHC. Conclusion: All the results imply that the accurate and reproducible method developed has high separation rate and enables the determination of 10 bioactive components in a single run for the quality control of CHC. PMID:24696551

High-resolution droplet-based fractionation of nano-LC separations onto microarrays for MALDI-MS analysis.

PubMed

Küster, Simon K; Pabst, Martin; Jefimovs, Konstantins; Zenobi, Renato; Dittrich, Petra S

2014-05-20

We present a robust droplet-based device, which enables the fractionation of ultralow flow rate nanoflow liquid chromatography (nano-LC) eluate streams at high frequencies and high peak resolution. This is achieved by directly interfacing the separation column to a micro T-junction, where the eluate stream is compartmentalized into picoliter droplets. This immediate compartmentalization prevents peak dispersion during eluate transport and conserves the chromatographic performance. Subsequently, nanoliter eluate fractions are collected at a rate of one fraction per second on a high-density microarray to retain the separation with high temporal resolution. Chromatographic separations of up to 45 min runtime can thus be archived on a single microarray possessing 2700 sample spots. The performance of this device is demonstrated by fractionating the separation of a tryptic digest of a known protein mixture onto the microarray chip and subsequently analyzing the sample archive using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Resulting peak widths are found to be significantly reduced compared to standard continuous flow spotting technologies as well as in comparison to a conventional nano-LC-electrospray ionization-mass spectrometry interface. Moreover, we demonstrate the advantage of our high-definition nanofractionation device by applying two different MALDI matrices to all collected fractions in an alternating fashion. Since the information that is obtained from a MALDI-MS measurement depends on the choice of MALDI matrix, we can extract complementary information from neighboring spots containing almost identical composition but different matrices.

Fractionalized Fermi liquid in a Kondo-Heisenberg model

DOE PAGES

Tsvelik, A. M.

2016-10-10

The Kondo-Heisenberg model is used as a controllable tool to demonstrate the existence of a peculiar metallic state with unbroken translational symmetry where the Fermi surface volume is not controlled by the total electron density. Here, I use a nonperturbative approach where the strongest interactions are taken into account by means of exact solution, and corrections are controllable. The resulting metallic state represents a fractionalized Fermi liquid where well defined quasiparticles coexist with gapped fractionalized collective excitations, in agreement with the general requirements formulated by T. Senthil et al. [Phys. Rev. Lett. 90, 216403 (2003)]. Furthermore, the system undergoes amore » phase transition to an ordered phase (charge density wave or superconducting), at the transition temperature which is parametrically small in comparison to the quasiparticle Fermi energy.« less

A validated high-performance liquid chromatographic method for the determination of moclobemide and its two metabolites in human plasma and application to pharmacokinetic studies.

PubMed

Plenis, Alina; Chmielewska, Aleksandra; Konieczna, Lucyna; Lamparczyk, Henryk

2007-09-01

A rapid and sensitive reversed-phase high-performance liquid chromatographic method (RP-HPLC) with ultraviolet detection has been developed for the determination of moclobemide and its metabolites, p-chloro-N-(-2-morpholinoethyl)benzamide N'-oxide (Ro 12-5637) and p-chloro-N-[2-(3-oxomorpholino)ethyl]-benzamide (Ro 12-8095), in human plasma. The assay was performed after single liquid-liquid extraction with dichloromethane at alkaline pH using phenacetin as the internal standard. Chromatographic separation was performed on a C(18) column using a mixture of acetonitrile and water (25:75, v/v), adjusted to pH 2.7 with ortho-phosphoric acid, as mobile phase. Spectrophotometric detection was performed at 239 nm. The method has been validated for accuracy, precision, selectivity, linearity, recovery and stability. The quantification limit for moclobemide and Ro 12-8095 was 10 ng/mL, and for Ro 12-5637 was 30 ng/mL. Linearity of the method was confirmed for the range 20-2500 ng/mL for moclobemide (r = 0.9998), 20-1750 ng/mL for Ro 12-8095 (r = 0.9996) and 30-350 ng/mL for Ro 12-5637 (r = 0.9991). Moreover, within-day and between-day precisions and accuracies of the method were established. The described method was successfully applied in pharmacokinetic studies of parent drug and its two metabolites after a single oral administration of 150 mg of moclobemide to 20 healthy volunteers. Copyright (c) 2007 John Wiley & Sons, Ltd.

High-performance liquid chromatographic method optimization for ondansetron assay in extemporaneous topical gel and in marketed products.

PubMed

Quamrun, Masuda; Mamoon, Rashid; Nasheed, Shams; Randy, Mullins

2014-01-01

The compounding and evaluation of ondansetron hydrochloride dihydrate topical gel, 2.5% w/w, were conducted in this study. The gelling agent was Carbopol 940. Ethanol 70% in purified water was used to dissolve the drug and disperse the gelling agent. A gel was formed by adding drops of 0.1 N sodium hydroxide solution. To assay this gel, we developed a simple and reproducible stability--indicating high-performance liquid chromatographic method. This method was validated for specificity, accuracy, and precision. The compounded gel was assayed in triplicate, and the average recovery was 98.3%. Ondansetron marketed products were analyzed for comparison with the compounded formulation. Assay, accuracy, and precision data of the compounded topical gel were comparable to the marketed products.

Liquid chromatographic method for determining the concentration of bisazir in water

USGS Publications Warehouse

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

1997-01-01

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

Development and Validation of Liquid Chromatographic Method for Estimation of Naringin in Nanoformulation

PubMed Central

Musmade, Kranti P.; Trilok, M.; Dengale, Swapnil J.; Bhat, Krishnamurthy; Reddy, M. S.; Musmade, Prashant B.; Udupa, N.

2014-01-01

A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC) method with UV detection has been developed and validated for quantification of naringin (NAR) in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by employing a C18 (250.0 × 4.6 mm, 5 μm) column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v) as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1). The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV) less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity. PMID:26556205

Apparatus for measuring the local void fraction in a flowing liquid containing a gas

DOEpatents

Dunn, P.F.

1979-07-17

The local void fraction in liquid containing a gas is measured by placing an impedance-variation probe in the liquid, applying a controlled voltage or current to the probe, and measuring the probe current or voltage. A circuit for applying the one electrical parameter and measuring the other includes a feedback amplifier that minimizes the effect of probe capacitance and a digitizer to provide a clean signal. Time integration of the signal provides a measure of the void fraction, and an oscilloscope display also shows bubble size and distribution.

Apparatus for measuring the local void fraction in a flowing liquid containing a gas

DOEpatents

Dunn, Patrick F.

1981-01-01

The local void fraction in liquid containing a gas is measured by placing an impedance-variation probe in the liquid, applying a controlled voltage or current to the probe, and measuring the probe current or voltage. A circuit for applying the one electrical parameter and measuring the other includes a feedback amplifier that minimizes the effect of probe capacitance and a digitizer to provide a clean signal. Time integration of the signal provides a measure of the void fraction, and an oscilloscope display also shows bubble size and distribution.

Application of an innovative design space optimization strategy to the development of liquid chromatographic methods to combat potentially counterfeit nonsteroidal anti-inflammatory drugs.

PubMed

Mbinze, J K; Lebrun, P; Debrus, B; Dispas, A; Kalenda, N; Mavar Tayey Mbay, J; Schofield, T; Boulanger, B; Rozet, E; Hubert, Ph; Marini, R D

2012-11-09

In the context of the battle against counterfeit medicines, an innovative methodology has been used to develop rapid and specific high performance liquid chromatographic methods to detect and determine 18 non-steroidal anti-inflammatory drugs, 5 pharmaceutical conservatives, paracetamol, chlorzoxazone, caffeine and salicylic acid. These molecules are commonly encountered alone or in combination on the market. Regrettably, a significant proportion of these consumed medicines are counterfeit or substandard, with a strong negative impact in countries of Central Africa. In this context, an innovative design space optimization strategy was successfully applied to the development of LC screening methods allowing the detection of substandard or counterfeit medicines. Using the results of a unique experimental design, the design spaces of 5 potentially relevant HPLC methods have been developed, and transferred to an ultra high performance liquid chromatographic system to evaluate the robustness of the predicted DS while providing rapid methods of analysis. Moreover, one of the methods has been fully validated using the accuracy profile as decision tool, and was then used for the quantitative determination of three active ingredients and one impurity in a common and widely used pharmaceutical formulation. The method was applied to 5 pharmaceuticals sold in the Democratic Republic of Congo. None of these pharmaceuticals was found compliant to the European Medicines Agency specifications. Copyright © 2012 Elsevier B.V. All rights reserved.

Catalytic two-stage coal hydrogenation process using extinction recycle of heavy liquid fraction

DOEpatents

MacArthur, J.B.; Comolli, A.G.; McLean, J.B.

1989-10-17

A process is described for catalytic two-stage hydrogenation and liquefaction of coal with selective extinction recycle of all heavy liquid fractions boiling above a distillation cut point of about 600--750 F to produce increased yields of low-boiling hydrocarbon liquid and gas products. In the process, the particulate coal feed is slurried with a process-derived liquid solvent normally boiling above about 650 F and fed into a first stage catalytic reaction zone operated at conditions which promote controlled rate liquefaction of the coal, while simultaneously hydrogenating the hydrocarbon recycle oils. The first stage reactor is maintained at 710--800 F temperature, 1,000--4,000 psig hydrogen partial pressure, and 10-90 lb/hr per ft[sup 3] catalyst space velocity. Partially hydrogenated material withdrawn from the first stage reaction zone is passed directly to the second stage catalytic reaction zone maintained at 760--860 F temperature for further hydrogenation and hydroconversion reactions. A 600--750 F[sup +] fraction containing 0--20 W % unreacted coal and ash solids is recycled to the coal slurrying step. If desired, the cut point lower boiling fraction can be further catalytically hydrotreated. By this process, the coal feed is successively catalytically hydrogenated and hydroconverted at selected conditions, to provide significantly increased yields of desirable low-boiling hydrocarbon liquid products and minimal production of hydrocarbon gases, and no net production of undesirable heavy oils and residuum materials. 2 figs.

Catalytic two-stage coal hydrogenation process using extinction recycle of heavy liquid fraction

DOEpatents

MacArthur, James B.; Comolli, Alfred G.; McLean, Joseph B.

1989-01-01

A process for catalytic two-stage hydrogenation and liquefaction of coal with selective extinction recycle of all heavy liquid fractions boiling above a distillation cut point of about 600.degree.-750.degree. F. to produce increased yields of low-boiling hydrocarbon liquid and gas products. In the process, the particulate coal feed is slurried with a process-derived liquid solvent normally boiling above about 650.degree. F. and fed into a first stage catalytic reaction zone operated at conditions which promote controlled rate liquefaction of the coal, while simultaneously hydrogenating the hydrocarbon recycle oils. The first stage reactor is maintained at 710.degree.-800.degree. F. temperature, 1000-4000 psig hydrogen partial pressure, and 10-90 lb/hr per ft.sup.3 catalyst space velocity. Partially hydrogenated material withdrawn from the first stage reaction zone is passed directly to the second stage catalytic reaction zone maintained at 760.degree.-860.degree. F. temperature for further hydrogenation and hydroconversion reactions. A 600.degree.-750.degree. F..sup.+ fraction containing 0-20 W % unreacted coal and ash solids is recycled to the coal slurrying step. If desired, the cut point lower boiling fraction can be further catalytically hydrotreated. By this process, the coal feed is successively catalytically hydrogenated and hydroconverted at selected conditions, to provide significantly increased yields of desirable low-boiling hydrocarbon liquid products and minimal production of hydrocarbon gases, and no net production of undesirable heavy oils and residuum materials.

Some high-performance liquid-chromatographic studies of the metabolism of aflatoxins by rat liver microsomal preparations.

PubMed Central

Neal, G E; Colley, P J

1978-01-01

The metabolism of aflatoxin B1 in vitro was examined in rat liver microsomal preparations. 2. H.p.l.c. (high-performance liquid-chromatographic) systems were used. A silica column was used to separate non-polar metabolites. A system utilizing a reversed-phase column which separates both poar and non-polar metabolites was also developed. 3. The principal metabolites of aflatoxin B1 found were aflatoxin M1, aflatoxin Q1 and a compound which co-chromatographed with a degradation product of aflatoxin B1 2,3-dihydrodiol. 4. The time course of metabolism of aflatoxin B1 by microsomal preparations isolated from control and phenobarbitone-pretreated rats was examined. The rate and extent of metabolism was greater with microsomal preparations from the latter. The formation of aflatoxin Q1 was enhanced 4--5-fold by phenobarbitone pretreatment, whereas the production of aflatoxin M1 was only increased 1--2-fold. The formation of the degradation product of aflatoxin B1 2,3-dihydrodiol was increased 4--5-fold by the pretreatment with phenobarbitone. 5. The microsomal metabolism of aflatoxins M1, P1 and Q1 was examined. Aflatoxin M1 apparently underwent very limited microsomal metabolism to more polar compounds. Aflatoxin P1 was not metabolized. The situation with aflatoxin Q1 was complicated in that it was metabolized in the absence of NADPH to an unidentified metabolite. Aflatoxin B1 appeared as a metabolite of aflatoxin Q1 only when NADPH was present, and the formation of more polar metabolites was also then observed. PMID:728090

Micellar liquid chromatographic determination of arbutin and hydroquinone in medicinal plant extracts and commercial cosmetic products.

PubMed

Thogchai, W; Liawruangrath, B

2013-06-01

A simple micellar liquid chromatographic (MLC) procedure for simultaneous determination of arbutin and hydroquinone in medicinal plant extracts and commercial cosmetic products was proposed. This method was developed and validated. The chromatographic conditions were also optimized. All analyses were performed at room temperature in an isocratic mode, using a mixture of 1% (v/v) acetonitrile and 0.006 mol L⁻¹ Brij 35 (pH 6.0) as a mobile phase. The flow rate was set at 1.0 mL min⁻¹. The analytical column was a 150 × 3.9 mm Nova-Pak C-18 column. The effluent from the analytical column was monitored by UV detection at 280 nm. Under the optimum conditions, arbutin and hydroquinone could be determined within a concentration range of 2-50 μg mL⁻¹ of arbutin, and hydroquinone was obtained with the regression equations; y = 0.045x + 0.042 (r² = 0.9923) and y = 0.091x + 0.050 (r² = 0.9930) respectively. The limits of detection were found to be 0.51 μg mL⁻¹ and 0.37 μg mL⁻¹ for arbutin and hydroquinone respectively. The proposed MLC method was applied for the determination of arbutin and hydroquinone contents in medicinal plant extracts and commercial cosmetic products. This proposed MLC method is thus suitable for routine analysis of arbutin and hydroquinone in the pharmaceutical formulations, cosmetic products and raw medicinal plant extracts. ICS © 2013 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Fast, simple and efficient salting-out assisted liquid-liquid extraction of naringenin from fruit juice samples prior to their enantioselective determination by liquid chromatography.

PubMed

Magiera, Sylwia; Kwietniowska, Ewelina

2016-11-15

In this study, an easy, simple and efficient method for the determination of naringenin enantiomers in fruit juices after salting-out-assisted liquid-liquid extraction (SALLE) and high-performance liquid chromatography (HPLC) with diode-array detection (DAD) was developed. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. After extraction, juice samples were incubated with hydrochloric acid in order to achieve hydrolysis of naringin to naringenin. The hydrolysis parameters were optimized by using a half-fraction factorial central composite design (CCD). After sample preparation, chromatographic separation was obtained on a Chiralcel® OJ-RH column using the mobile phase consisting of 10mM aqueous ammonium acetate:methanol:acetonitrile (50:30:20; v/v/v) with detection at 288nm. The average recovery of the analyzed compounds ranged from 85.6 to 97.1%. The proposed method was satisfactorily used for the determination of naringenin enantiomers in various fruit juices samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

High-performance liquid chromatographic determination of loxoprofen and its diastereomeric alcohol metabolites in biological fluids by fluorescence labelling with 4-bromomethyl-6,7-methylenedioxycoumarin.

PubMed

Naganuma, H; Kawahara, Y

1990-09-14

A simple and sensitive high-performance liquid chromatographic procedure to determine loxoprofen and its diastereomeric alcohol metabolites in biological specimens is described. The analysis involves liquid-liquid extraction with benzene, pre-column derivatization with a highly fluorogenic reagent, 4-bromomethyl-6,7-methylenedioxycoumarin (BrMDC) and subsequent separation on a reversed-phase column. Loxoprofen, its pharmacologically active metabolite, trans-alcohol, and less active cis-alcohol were completely separated within 20 min with a mobile phase of 55% of aqueous acetonitrile containing acetic acid. Any endogenous substances do not interfere in the analysis of either plasma or urine samples. The quantitation limit was 0.01 micrograms/ml for human plasma and 0.05 micrograms/ml for urine. The method was applied to a pharmacokinetic study in healthy human subjects who had received 60 mg of loxoprofen sodium.

Column Liquid Chromatography.

ERIC Educational Resources Information Center

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,…

Skin whitening and anti-corrugation activities of glycoprotein fractions from liquid extracts of boiled sea cucumber.

PubMed

Kim, So Jung; Park, So Yun; Hong, Sun-Mee; Kwon, Eun-Hye; Lee, Taek-Kyun

2016-10-01

To determine skin whitening and wrinkle improvement efficacy, glycoprotein fractions were extracted from liquid extracts of boiled sea cucumber and their effects on tyrosine and elastase inhibitory activities were assayed. Fractions above and below 50 kDa (>50 kDa and <50 kDa) were extracted via a series of steps involving: boiling, filtering, desalting and freeze drying. Cytotoxicity, skin whitening and wrinkle-removing effects of boiled liquid were determined. Our MTT data showed that neither glycoprotein fraction of boiled liquid induces cellular cytotoxicity up to a concentration of 10 mg/mL treatment of the mouse melanoma cell line, B16F10, with 10 mg/mL >50 kDa enhanced tyrosinase and elastase inhibitory activities by 50.84% and 28.78%, respectively. Correlations of the >50 kDa concentration with tyrosinase inhibitory (R2 = 0.968) and elastase inhibitory (R2 = 0.983) efficacy were significant. >50 kDa glycoprotein fraction isolated from liquid extracts of boiled sea cucumber, which can serve as a functional cosmetic ingredient for whitening and wrinkle improvement of skin. Copyright © 2016 Hainan Medical University. Production and hosting by Elsevier B.V. All rights reserved.

High-performance Liquid Chromatographic Ultraviolet Detection of Nilotinib in Human Plasma from Patients with Chronic Myelogenous Leukemia, and Comparison with Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Nakahara, Ryosuke; Satho, Yuhki; Itoh, Hiroki

2016-11-01

A method for determining nilotinib concentration in human plasma is proposed using high-performance liquid chromatography and ultraviolet detection. Nilotinib and the internal standard dasatinib were separated using a mobile phase of 0.5% Na 2 PO 4 H 2 O (pH 2.5)-acetonitrile-methanol (55:25:20, v/v/v) on a Capcell Pak C18 MG II column (250 × 4.6 mm) at a flow rate of 1.0 ml/min, and ultraviolet measurement at 250 nm. The calibration curve exhibited linearity over the nilotinib concentration range of 50-2,500 ng/ml at 250 nm, with relative standard deviations (n = 5) of 7.1%, 2.5%, and 2.9% for 250, 1,500, and 2,500 ng/ml, respectively. The detection limit for nilotinib was 5 ng/ml due to three blank determinations (ρ = 3). This method was successfully applied to assaying nilotinib in human plasma samples from patients with chronic myelogenous leukemia. In addition, we compared the results with those measured by liquid chromatography-tandem mass spectrometry (LC-MS/MS) at BML, Inc. (a commercial laboratory). A strong correlation was observed between the nilotinib concentrations measured by our high-performance liquid chromatographic method and those obtained by LC/MS-MS (r 2 = 0.988, P < 0.01). © 2016 Wiley Periodicals, Inc.

Characterization of Gas Chromatographic Liquid Phases Using McReynolds Constants. An Experiment for Instrumental Analysis Laboratory.

ERIC Educational Resources Information Center

Erskine, Steven R.; And Others

1986-01-01

Describes a laboratory experiment that is designed to aid in the understanding of the fundamental process involved in gas chromatographic separations. Introduces the Kovats retention index system for use by chemistry students to establish criteria for the optimal selection of gas chromatographic stationary phases. (TW)

An Eight-Month Sample of Marine Stratocumulus Cloud Fraction, Albedo, and Integrated Liquid Water.

NASA Astrophysics Data System (ADS)

Fairall, C. W.; Hare, J. E.; Snider, J. B.

1990-08-01

As part of the First International Satellite Cloud Climatology Regional Experiment (FIRE), a surface meteorology and shortwave/longwave irradiance station was operated in a marine stratocumulus regime on the northwest tip of San Nicolas island off the coast of Southern California. Measurements were taken from March through October 1987, including a FIRE Intensive Field Operation (IFO) held in July. Algorithms were developed to use the longwave irradiance data to estimate fractional cloudiness and to use the shortwave irradiance to estimate cloud albedo and integrated cloud liquid water content. Cloud base height is estimated from computations of the lifting condensation level. The algorithms are tested against direct measurements made during the IFO; a 30% adjustment was made to the liquid water parameterization. The algorithms are then applied to the entire database. The stratocumulus clouds over the island are found to have a cloud base height of about 400 m, an integrated liquid water content of 75 gm2, a fractional cloudiness of 0.95, and an albedo of 0.55. Integrated liquid water content rarely exceeds 350 g m2 and albedo rarely exceeds 0.90 for stratocumulus clouds. Over the summer months, the average cloud fraction shows a maximum at sunrise of 0.74 and a minimum at sunset of 0.41. Over the same period, the average cloud albedo shows a maximum of 0.61 at sunrise and a minimum of 0.31 a few hours after local noon (although the estimate is more uncertain because of the extreme solar zenith angle). The use of joint frequency distributions of fractional cloudiness with solar transmittance or cloud base height to classify cloud types appears to be useful.

Note on the chromatographic analyses of marine polyunsaturated fatty acids

USGS Publications Warehouse

Schultz, D.M.; Quinn, J.G.

1977-01-01

Gas-liquid chromatography was used to study the effects of saponification/methylation and thin-layer chromatographic isolation on the analyses of polyunsaturated fatty acids. Using selected procedures, the qualitative and quantitative distribution of these acids in marine organisms can be determined with a high degree of accuracy. ?? 1977 Springer-Verlag.

Fiber-based monolithic columns for liquid chromatography.

PubMed

Ladisch, Michael; Zhang, Leyu

2016-10-01

Fiber-based monoliths for use in liquid chromatographic separations are defined by columns packed with aligned fibers, woven matrices, or contiguous fiber structures capable of achieving rapid separations of proteins, macromolecules, and low molecular weight components. A common denominator and motivating driver for this approach, first initiated 25 years ago, was reducing the cost of bioseparations in a manner that also reduced residence time of retained components while achieving a high ratio of mass to momentum transfer. This type of medium, when packed into a liquid chromatography column, minimized the fraction of stagnant liquid and resulted in a constant plate height for non-adsorbing species. The uncoupling of dispersion from eluent flow rate enabled the surface chemistry of the stationary phase to be considered separately from fluid transport phenomena and pointed to new ways to apply chemistry for the engineering of rapid bioseparations. This paper addresses developments and current research on fiber-based monoliths and explains how the various forms of this type of chromatographic stationary phase have potential to provide new tools for analytical and preparative scale separations. The different stationary phases are discussed, and a model that captures the observed constant plate height as a function of mobile phase velocity is reviewed. Methods that enable hydrodynamically stable fiber columns to be packed and operated over a range of mobile phase flow rates, together with the development of new fiber chemistries, are shown to provide columns that extend the versatility of liquid chromatography using monoliths, particularly at the preparative scale. Graphical Abstract Schematic representation of a sample mixture being separated by a rolled-stationary phase column, resulting separated peaks shown in the chromatogram.

Analysis of amide compounds in different parts of Piper ovatum Vahl by high-performance liquid chromatographic

PubMed Central

Silva, Daniel R.; Brenzan, Mislaine A.; Kambara, Lauro M.; Cortez, Lucia E. R.; Cortez, Diógenes A. G.

2013-01-01

Background: Piper ovatum (Piperaceae) has been used in traditional medicine for the treatment of inflammations and as an analgesic. Previous studies have showed important biological activities of the extracts and amides from P. ovatum leaves. Objective: In this study, a high-performance liquid chromatographic (HPLC) method was developed and validated for quantitative determination of the amides in different parts of Piper ovatum. Materials and Methods: The analysis was carried out on a Metasil ODS column (150 × 4.6 mm, 5μm) at room temperature. HPLC conditions were as follows: acetonitrile (A), and water (B), 1.0% acetic acid. The gradient elution used was 0–30 min, 0-60% A; 30–40 min, 60% A. Flow rate used was 1.0mL/min, and detection at 280nm. Results: The validation using piperlonguminine, as the standard, demonstrated that the method shows linearity (linear correlation coefficient = 0.998), precision (relative standard deviation <5%) and accuracy (mean recovery = 103.78%) in the concentration range 31.25 – 500μg/mL. The limit of detection and quantification were 1.21 and 4.03μg/mL, respectively. This method allowed the identification and quantification of piperlonguminine and piperovatine in the hydroethanolic extracts of P. ovatum obtained from the leaves, stems and roots. All the extracts showed the same chromatographic profile. The leaves and roots contained the highest concentrations of piperlonguminine and the stems and leaves showed the most concentrations of piperovatine. Conclusion: This HPLC method is suitable for routine quantitative analysis of amides in extracts of Piper ovatum and phytopharmaceuticals containing this herb. PMID:24174818

Gas chromatographic column for the Viking 1975 molecular analysis experiment

NASA Technical Reports Server (NTRS)

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

1975-01-01

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

Direct Contact Heat Exchange Interfacial Phenomena for Liquid Metal Reactors: Part II - Void Fraction

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

Abdulla, S.; Liu, X.; Anderson, M.H.

One concept being considered for steam generation in innovative nuclear reactor applications, involves water coming into direct contact with a circulating molten metal. The vigorous agitation of the two fluids, the direct liquid-liquid contact and the consequent large interfacial area can give rise to large heat transfer coefficients and rapid steam generation. For an optimum design of such direct contact heat exchange and vaporization systems, detailed knowledge is necessary of the various flow regimes, interfacial transport phenomena, heat transfer and operational stability. In order to investigate the interfacial transport phenomena, heat transfer and operational stability of direct liquid-liquid contact, amore » series of experiments are being performed in a 1-d test facility at Argonne National Laboratory and a 2-d experimental facility at UW-Madison. Each of the experimental facilities primarily consist of a liquid-metal melt chamber, heated test section (10 cm diameter tube for 1-d facility and 10 cm 50 cm rectangle for 2-d facility), water injection system and steam suppression tank. This paper is part II which, primarily addresses results and analysis of a set of preliminary experiments and void fraction measurements conducted in the 2-d facility at UW-Madison, part I deals with the heat transfer in the 1-d test facility at Argonne National Laboratory. A real-time high energy X-ray imaging system was developed and utilized to visualize the multiphase flow and measure line-average local void fractions, time-dependent void fraction distribution as well as estimates of the vapor bubble sizes and velocities. These measurements allowed us to determine the volumetric heat transfer coefficient and gain insight into the local heat transfer mechanisms. In this study, the images were captured at frame rates of 100 fps with spatial resolution of about 7 mm with a full-field view of a 15 cm square and five different positions along the test section height. The full

Robotic solid phase extraction and high performance liquid chromatographic analysis of ranitidine in serum or plasma.

PubMed

Lloyd, T L; Perschy, T B; Gooding, A E; Tomlinson, J J

1992-01-01

A fully automated assay for the analysis of ranitidine in serum and plasma, with and without an internal standard, was validated. It utilizes robotic solid phase extraction with on-line high performance liquid chromatographic (HPLC) analysis. The ruggedness of the assay was demonstrated over a three-year period. A Zymark Py Technology II robotic system was used for serial processing from initial aspiration of samples from original collection containers, to final direct injection onto the on-line HPLC system. Automated serial processing with on-line analysis provided uniform sample history and increased productivity by freeing the chemist to analyse data and perform other tasks. The solid phase extraction efficiency was 94% throughout the assay range of 10-250 ng/mL. The coefficients of variation for within- and between-day quality control samples ranged from 1 to 6% and 1 to 5%, respectively. Mean accuracy for between-day standards and quality control results ranged from 97 to 102% of the respective theoretical concentrations.

Group-type hydrocarbon standards for high-performance liquid chromatographic analysis of middistillate fuels

NASA Technical Reports Server (NTRS)

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

1984-01-01

A new high-performance liquid chromatographic (HPLC) method for group-type analysis of middistillate fuels is described. It uses a refractive index detector and standards that are prepared by reacting a portion of the fuel sample with sulfuric acid. A complete analysis of a middistillate fuel for saturates and aromatics (including the preparation of the standard) requires about 15 min if standards for several fuels are prepared simultaneously. From model fuel studies, the method was found to be accurate to within 0.4 vol% saturates or aromatics, and provides a precision of + or - 0.4 vol%. Olefin determinations require an additional 15 min of analysis time. However, this determination is needed only for those fuels displaying a significant olefin response at 200 nm (obtained routinely during the saturated/aromatics analysis procedure). The olefin determination uses the responses of the olefins and the corresponding saturates, as well as the average value of their refractive index sensitivity ratios (1.1). Studied indicated that, although the relative error in the olefins result could reach 10 percent by using this average sensitivity ratio, it was 5 percent for the fuels used in this study. Olefin concentrations as low as 0.1 vol% have been determined using this method.

An Interactive Computer Program for Simulating the Effects of Olivine Fractionation from Basaltic and Ultrabasic Liquids.

ERIC Educational Resources Information Center

Pearce, Thomas H.

1983-01-01

Describes interactive computer program (listing available from author) which simulates olivine fractionation from basaltic/ultrabasic liquid. The menu-driven nature of the program (for Apple II microcomputer) allows students to select ideal Rayleigh fractionation or equilibrium crystallization. (JN)

A validated chiral liquid chromatographic method for the enantiomeric separation of safinamide mesilate, a new anti-Parkinson drug.

PubMed

Zhang, Kai; Xue, Na; Shi, Xiaowei; Liu, Weina; Meng, Jing; Du, Yumin

2011-04-28

A enantioselective reversed-phase high performance liquid chromatographic method was developed for the enantiomeric resolution of safinamide mesilate, 2(S)-[4-(3-fluorobenzyloxy)benzylamino] propionamide methanesulfonate, a neuroprotectant with antiparkinsonian and anticonvulsant activity for the treatment of Parkinson disease. The enantiomers of safinamide mesilate were baseline resolved on a Chiralcel OD-RH (150mm×4.6mm, 5μm) column using a mobile phase system containing 300mM sodium di-hydrogen phosphate buffer (pH 3.0):methanol:acetonitrile (65:25:10, v/v/v). The resolution between the enantiomers was not less than 3.0. The pH value of buffer solution in the mobile phase has played a key role in enhancing chromatographic efficiency and resolution between the enantiomers. The developed method was validated and proved to be robust. The limit of detection and limit of quantification of (R)-enantiomer were found to be 15 and 50ng/mL, respectively, for 20μL injection volume. The percentage recovery of (R)-enantiomer was ranged from 94.2 to 103.7 in bulk drug samples of safinamide mesilate. The sample solution and mobile phase were found to be stable at least for 48h. The final optimized method was successfully applied to separate (R)-enantiomer from safinamide mesilate and was proven to be reproducible and accurate for the quantitative determination of (R)-enantiomer in bulk drugs. Copyright © 2010 Elsevier B.V. All rights reserved.

Characterization of taste-active fractions in red wine combining HPLC fractionation, sensory analysis and ultra performance liquid chromatography coupled with mass spectrometry detection.

PubMed

Sáenz-Navajas, María-Pilar; Ferreira, Vicente; Dizy, Marta; Fernández-Zurbano, Purificación

2010-07-19

Five Tempranillo wines exhibiting marked differences in taste and/or astringency were selected for the study. In each wine the non-volatile extract was obtained by freeze-drying and further liquid extraction in order to eliminate remaining volatile compounds. This extract was fractionated by semipreparative C18-reverse phase-high performance liquid chromatography (C18-RP-HPLC) into nine fractions which were freeze-dried, reconstituted with water and sensory assessed for taste attributes and astringency by a specifically trained sensory panel. Results have shown that wine bitterness and astringency cannot be easily related to the bitter and astringent character of the HPLC fractions, what can be due to the existence of perceptual and physicochemical interactions. While the bitter character of the bitterest fractions may be attributed to some flavonols (myricetin, quercetin and their glycosides) the development of a sensitive UPLC-MS method to quantify astringent compounds present in wines has made it possible to demonstrate that proanthocyanidins monomers, dimers, trimers and tetramers, both galloylated or non-galloylated are not relevant compounds for the perceived astringency of the fractions, while cis-aconitic acid, and secondarily vainillic, and syringic acids and ethyl syringate, are the most important molecules driving astringency in two of the fractions (F5 and F6). The identity of the chemicals responsible for the astringency of the third fraction could be assigned to some proanthocyanidins (higher than the tetramer) capable to precipitate with ovalbumin. 2010 Elsevier B.V. All rights reserved.

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

USGS Publications Warehouse

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

1984-01-01

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

Chromatographic column evaluation for the untargeted profiling of glucosinolates in cauliflower by means of ultra-high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Montone, Carmela Maria; Piovesana, Susy; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2018-03-01

The untargeted profiling is a promising approach for the characterization of secondary metabolites in biological matrices. Thanks to the recent rapid development of high-resolution mass spectrometry (HRMS) instrumentations, the number of applications by untargeted approaches for biological samples profiling has widely increased in the recent years. Despite the high potentialities of HRMS, however, a major issue in natural products analysis often arises in the upstream process of compounds separation. A separation technique is necessary to avoid phenomena such as signal suppression, and it is especially needed in the presence of isomeric metabolites, which are otherwise indistinguishable. Glucosinolates (GLSs), a group of secondary metabolites widely distributed among plants, resulted to be associated to the prevention of some serious diseases, such as cancer. This led to the development of several methods for the analysis of GLSs in vegetables tissues. The issue of GLSs chromatographic separation has been widely studied in the past because of the difficulty in the analysis of this highly polar and variable class of compounds. Several alternatives to reversed phase (RP) chromatography, sometimes not compatible with the coupling of liquid chromatography with mass spectrometry, have been tested for the analysis of intact GLSs. However, the availability of new stationary phases, in the last years, could allow the re-evaluation of RP chromatography for the analysis of intact GLSs. In this work, a thorough evaluation of four RP chromatographic columns for the analysis of GLSs in cauliflower (Brassica oleracea L. var. botrytis) extracts by an ultra-high performance liquid chromatographic system coupled via electrospray source to a hybrid quadrupole-Orbitrap mass spectrometer is presented. The columns tested were the following: one column Luna Omega polar C 18 , one column Kinetex Biphenyl, one column Kinetex core-shell XB-C 18 , two columns Kinetex core-shell XB-C 18

Simple automatic strategy for background drift correction in chromatographic data analysis.

PubMed

Fu, Hai-Yan; Li, He-Dong; Yu, Yong-Jie; Wang, Bing; Lu, Peng; Cui, Hua-Peng; Liu, Ping-Ping; She, Yuan-Bin

2016-06-03

Chromatographic background drift correction, which influences peak detection and time shift alignment results, is a critical stage in chromatographic data analysis. In this study, an automatic background drift correction methodology was developed. Local minimum values in a chromatogram were initially detected and organized as a new baseline vector. Iterative optimization was then employed to recognize outliers, which belong to the chromatographic peaks, in this vector, and update the outliers in the baseline until convergence. The optimized baseline vector was finally expanded into the original chromatogram, and linear interpolation was employed to estimate background drift in the chromatogram. The principle underlying the proposed method was confirmed using a complex gas chromatographic dataset. Finally, the proposed approach was applied to eliminate background drift in liquid chromatography quadrupole time-of-flight samples used in the metabolic study of Escherichia coli samples. The proposed method was comparable with three classical techniques: morphological weighted penalized least squares, moving window minimum value strategy and background drift correction by orthogonal subspace projection. The proposed method allows almost automatic implementation of background drift correction, which is convenient for practical use. Copyright © 2016 Elsevier B.V. All rights reserved.

Methods for estimating properties of hydrocarbons comprising asphaltenes based on their solubility

DOEpatents

Schabron, John F.; Rovani, Jr., Joseph F.

2016-10-04

Disclosed herein is a method of estimating a property of a hydrocarbon comprising the steps of: preparing a liquid sample of a hydrocarbon, the hydrocarbon having asphaltene fractions therein; precipitating at least some of the asphaltenes of a hydrocarbon from the liquid sample with one or more precipitants in a chromatographic column; dissolving at least two of the different asphaltene fractions from the precipitated asphaltenes during a successive dissolution protocol; eluting the at least two different dissolved asphaltene fractions from the chromatographic column; monitoring the amount of the fractions eluted from the chromatographic column; using detected signals to calculate a percentage of a peak area for a first of the asphaltene fractions and a peak area for a second of the asphaltene fractions relative to the total peak areas, to determine a parameter that relates to the property of the hydrocarbon; and estimating the property of the hydrocarbon.

CN-GELFrEE - Clear Native Gel-eluted Liquid Fraction Entrapment Electrophoresis

PubMed Central

Skinner, Owen S.; Do Vale, Luis H. F.; Catherman, Adam D.; Havugimana, Pierre C.; Valle de Sousa, Marcelo; Domont, Gilberto B.; Kelleher, Neil L.; Compton, Philip D.

2016-01-01

Protein complexes perform an array of crucial cellular functions. Elucidating their non-covalent interactions and dynamics is paramount for understanding the role of complexes in biological systems. While the direct characterization of biomolecular assemblies has become increasingly important in recent years, native fractionation techniques that are compatible with downstream analysis techniques, including mass spectrometry, are necessary to further expand these studies. Nevertheless, the field lacks a high-throughput, wide-range, high-recovery separation method for native protein assemblies. Here, we present clear native gel-eluted liquid fraction entrapment electrophoresis (CN-GELFrEE), which is a novel separation modality for non-covalent protein assemblies. CN-GELFrEE separation performance was demonstrated by fractionating complexes extracted from mouse heart. Fractions were collected over 2 hr and displayed discrete bands ranging from ~30 to 500 kDa. A consistent pattern of increasing molecular weight bandwidths was observed, each ranging ~100 kDa. Further, subsequent reanalysis of native fractions via SDS-PAGE showed molecular-weight shifts consistent with the denaturation of protein complexes. Therefore, CN-GELFrEE was proved to offer the ability to perform high-resolution and high-recovery native separations on protein complexes from a large molecular weight range, providing fractions that are compatible with downstream protein analyses. PMID:26967310

A New Void Fraction Measurement Method for Gas-Liquid Two-Phase Flow in Small Channels

PubMed Central

Li, Huajun; Ji, Haifeng; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing; Wu, Guohua

2016-01-01

Based on a laser diode, a 12 × 6 photodiode array sensor, and machine learning techniques, a new void fraction measurement method for gas-liquid two-phase flow in small channels is proposed. To overcome the influence of flow pattern on the void fraction measurement, the flow pattern of the two-phase flow is firstly identified by Fisher Discriminant Analysis (FDA). Then, according to the identification result, a relevant void fraction measurement model which is developed by Support Vector Machine (SVM) is selected to implement the void fraction measurement. A void fraction measurement system for the two-phase flow is developed and experiments are carried out in four different small channels. Four typical flow patterns (including bubble flow, slug flow, stratified flow and annular flow) are investigated. The experimental results show that the development of the measurement system is successful. The proposed void fraction measurement method is effective and the void fraction measurement accuracy is satisfactory. Compared with the conventional laser measurement systems using standard laser sources, the developed measurement system has the advantages of low cost and simple structure. Compared with the conventional void fraction measurement methods, the proposed method overcomes the influence of flow pattern on the void fraction measurement. This work also provides a good example of using low-cost laser diode as a competent replacement of the expensive standard laser source and hence implementing the parameter measurement of gas-liquid two-phase flow. The research results can be a useful reference for other researchers’ works. PMID:26828488

A New Void Fraction Measurement Method for Gas-Liquid Two-Phase Flow in Small Channels.

PubMed

Li, Huajun; Ji, Haifeng; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing; Wu, Guohua

2016-01-27

Based on a laser diode, a 12 × 6 photodiode array sensor, and machine learning techniques, a new void fraction measurement method for gas-liquid two-phase flow in small channels is proposed. To overcome the influence of flow pattern on the void fraction measurement, the flow pattern of the two-phase flow is firstly identified by Fisher Discriminant Analysis (FDA). Then, according to the identification result, a relevant void fraction measurement model which is developed by Support Vector Machine (SVM) is selected to implement the void fraction measurement. A void fraction measurement system for the two-phase flow is developed and experiments are carried out in four different small channels. Four typical flow patterns (including bubble flow, slug flow, stratified flow and annular flow) are investigated. The experimental results show that the development of the measurement system is successful. The proposed void fraction measurement method is effective and the void fraction measurement accuracy is satisfactory. Compared with the conventional laser measurement systems using standard laser sources, the developed measurement system has the advantages of low cost and simple structure. Compared with the conventional void fraction measurement methods, the proposed method overcomes the influence of flow pattern on the void fraction measurement. This work also provides a good example of using low-cost laser diode as a competent replacement of the expensive standard laser source and hence implementing the parameter measurement of gas-liquid two-phase flow. The research results can be a useful reference for other researchers' works.

One input-class and two input-class classifications for differentiating olive oil from other edible vegetable oils by use of the normal-phase liquid chromatography fingerprint of the methyl-transesterified fraction.

PubMed

Jiménez-Carvelo, Ana M; Pérez-Castaño, Estefanía; González-Casado, Antonio; Cuadros-Rodríguez, Luis

2017-04-15

A new method for differentiation of olive oil (independently of the quality category) from other vegetable oils (canola, safflower, corn, peanut, seeds, grapeseed, palm, linseed, sesame and soybean) has been developed. The analytical procedure for chromatographic fingerprinting of the methyl-transesterified fraction of each vegetable oil, using normal-phase liquid chromatography, is described and the chemometric strategies applied and discussed. Some chemometric methods, such as k-nearest neighbours (kNN), partial least squared-discriminant analysis (PLS-DA), support vector machine classification analysis (SVM-C), and soft independent modelling of class analogies (SIMCA), were applied to build classification models. Performance of the classification was evaluated and ranked using several classification quality metrics. The discriminant analysis, based on the use of one input-class, (plus a dummy class) was applied for the first time in this study. Copyright © 2016 Elsevier Ltd. All rights reserved.

High-performance liquid chromatographic analysis of as-synthesised N,N'-dimethylformamide-stabilised gold nanoclusters product

NASA Astrophysics Data System (ADS)

Xie, Shunping; Paau, Man Chin; Zhang, Yan; Shuang, Shaomin; Chan, Wan; Choi, Martin M. F.

2012-08-01

Reverse-phase high-performance liquid chromatographic (RP-HPLC) separation and analysis of polydisperse water-soluble gold nanoclusters (AuNCs) stabilised with N,N'-dimethylformamide (DMF) were investigated. Under optimal elution gradient conditions, the separation of DMF-AuNCs was monitored by absorption and fluorescence spectroscopy. The UV-vis spectral characteristics of the separated DMF-AuNCs have been captured and they do not possess distinct surface plasmon resonance bands, indicating that all DMF-AuNCs are small AuNCs. The photoluminescence emission spectra of the separated DMF-AuNCs are in the blue-light region. Moreover, cationic DMF-AuNCs are for the first time identified by ion chromatography. Our proposed RP-HPLC methodology has been successfully applied to separate AuNCs of various Au atoms as well as DMF-stabilised ligands. Finally, the composition of the separated DMF-AuNCs was confirmed by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and electrospray ionisation mass spectrometry, proving that the as-synthesised DMF-AuNCs product consists of Au10+, Au10, Au11, Au12, Au13, and Au14 NCs stabilised with various numbers of DMF ligands.Reverse-phase high-performance liquid chromatographic (RP-HPLC) separation and analysis of polydisperse water-soluble gold nanoclusters (AuNCs) stabilised with N,N'-dimethylformamide (DMF) were investigated. Under optimal elution gradient conditions, the separation of DMF-AuNCs was monitored by absorption and fluorescence spectroscopy. The UV-vis spectral characteristics of the separated DMF-AuNCs have been captured and they do not possess distinct surface plasmon resonance bands, indicating that all DMF-AuNCs are small AuNCs. The photoluminescence emission spectra of the separated DMF-AuNCs are in the blue-light region. Moreover, cationic DMF-AuNCs are for the first time identified by ion chromatography. Our proposed RP-HPLC methodology has been successfully applied to separate AuNCs of

Assessing the varietal origin of extra-virgin olive oil using liquid chromatography fingerprints of phenolic compound, data fusion and chemometrics.

PubMed

Bajoub, Aadil; Medina-Rodríguez, Santiago; Gómez-Romero, María; Ajal, El Amine; Bagur-González, María Gracia; Fernández-Gutiérrez, Alberto; Carrasco-Pancorbo, Alegría

2017-01-15

High Performance Liquid Chromatography (HPLC) with diode array (DAD) and fluorescence (FLD) detection was used to acquire the fingerprints of the phenolic fraction of monovarietal extra-virgin olive oils (extra-VOOs) collected over three consecutive crop seasons (2011/2012-2013/2014). The chromatographic fingerprints of 140 extra-VOO samples processed from olive fruits of seven olive varieties, were recorded and statistically treated for varietal authentication purposes. First, DAD and FLD chromatographic-fingerprint datasets were separately processed and, subsequently, were joined using "Low-level" and "Mid-Level" data fusion methods. After the preliminary examination by principal component analysis (PCA), three supervised pattern recognition techniques, Partial Least Squares Discriminant Analysis (PLS-DA), Soft Independent Modeling of Class Analogies (SIMCA) and K-Nearest Neighbors (k-NN) were applied to the four chromatographic-fingerprinting matrices. The classification models built were very sensitive and selective, showing considerably good recognition and prediction abilities. The combination "chromatographic dataset+chemometric technique" allowing the most accurate classification for each monovarietal extra-VOO was highlighted. Copyright © 2016 Elsevier Ltd. All rights reserved.

Lignin Depolymerisation and Lignocellulose Fractionation by Solvated Electrons in Liquid Ammonia.

PubMed

Prinsen, Pepijn; Narani, Anand; Rothenberg, Gadi

2017-03-09

We explored the depolymerisation of several lignins in liquid ammonia at relatively high temperatures and pressures (120 °C and 88 bar). Five different lignins were tested: Indulin AT kraft, Protobind 1000 soda, wheat straw organosolv, poplar organosolv and elephant grass-milled wood lignin (EG MWL). In pure liquid ammonia, all lignins underwent slow incorporation of nitrogen into their structure, resulting in higher molecular weight and polydispersity index. Subsequently, we show a reductive depolymerisation by solvated electrons at room temperature by adding sodium metal to the liquid ammonia without any external hydrogen donor. The netto yields of bio-oil are low for technical lignins (10-23 %), but with higher yields of alkylphenols. In the case of native EG MWL, netto yields of 40 % bio-oil were achieved. Finally, when the room temperature method was applied to poplar wood fibre, we observe improved delignification upon the addition of sodium compared to poplar wood fractionation in pure liquid ammonia. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of pore size distributions of porous chromatographic adsorbents by inverse size-exclusion chromatography.

PubMed

Yao, Yan; Lenhoff, Abraham M

2004-05-28

The macroscopic properties of porous chromatographic adsorbents are directly influenced by the pore structure, with the pore size distribution (PSD) playing a major role beyond simply the mean pore size. Inverse size-exclusion chromatography (ISEC), a widely used chromatographic method for determining the PSD of porous media, provides more relevant information on liquid chromatographic materials in situ than traditional methods, such as gas sorption and mercury intrusion. The fundamentals and applications of ISEC in the characterization of the pore structure are reviewed. The description of the probe solutes and the pore space, as well as theoretical models for deriving the PSD from solute partitioning behavior, are discussed. Precautions to ensure integrity of the experiments are also outlined, including accounting for probe polydispersity and minimization of solute-adsorbent interactions. The results that emerge are necessarily model-dependent, but ISEC nonetheless represents a powerful and non-destructive source of quantitative pore structure information that can help to elucidate chromatographic performance observations covering both retention and rate aspects.

Ionic liquids in chromatographic and electrophoretic techniques: toward additional improvements in the separation of natural compounds

PubMed Central

Freire, Carmen S. R.; Coutinho, João A. P.; Silvestre, Armando J. D.; Freire, Mara G.

2016-01-01

Due to their unique properties, in recent years, ionic liquids (ILs) have been largely investigated in the field of analytical chemistry. Particularly during the last sixteen years, they have been successfully applied in the chromatographic and electrophoretic analysis of value-added compounds extracted from biomass. Considering the growing interest in the use of ILs in this field, this critical review provides a comprehensive overview on the improvements achieved using ILs as constituents of mobile or stationary phases in analytical techniques, namely in capillary electrophoresis and its different modes, in high performance liquid chromatography, and in gas chromatography, for the separation and analysis of natural compounds. The impact of the IL chemical structure and the influence of secondary parameters, such as the IL concentration, temperature, pH, voltage and analysis time (when applied), are also critically addressed regarding the achieved separation improvements. Major conclusions on the role of ILs in the separation mechanisms and the performance of these techniques in terms of efficiency, resolution and selectivity are provided. Based on a critical analysis of all published results, some target-oriented ILs are suggested. Finally, current drawbacks and future challenges in the field are highlighted. In particular, the design and use of more benign and effective ILs as well as the development of integrated (and thus more sustainable) extraction–separation processes using IL aqueous solutions are suggested within a green chemistry perspective. PMID:27667965

Liquid chromatographic method for the simultaneous determination of cefalexin and trimethoprim in dog plasma and application to the pharmacokinetic studies of a coformulated preparation.

PubMed

Qi, Meiling; Wang, Peng; Sun, Ping; Liu, Xia

2006-03-07

A liquid chromatographic method is described for the simultaneous determination of cefalexin and trimethoprim in dog plasma. A simple protein precipitation procedure was adopted for the sample preparation with satisfactory extraction recoveries for both analytes. Chromatographic separation of the analytes was achieved on a C(18) column using a mixture of 2 mol/l formate buffer (pH 3.5), methanol and acetonitrile (22:7:7, v/v/v) containing a 0.002 mol/l sodium dodecyl sulfate as mobile phase and detection was performed at 240 nm. The linearity was obtained over the concentration ranges of 1.0-100.0 microg/ml for cefalexin and 0.5-50.0 microg/ml for trimethoprim. For each level of QC samples including the lower limit of quantification, both inter- and intra-day precisions (R.S.D.) were < or =14.0% for cefalexin and < or =11.4% for trimethoprim, and accuracy (RE) was -1.4% for cefalexin and -3.0% for trimethoprim. The present LC method was successfully applied to the pharmacokinetic studies of coformulated cefalexin dispersible tablets after oral administration to beagle dogs.

The Development and Validation of Novel, Simple High-Performance Liquid Chromatographic Method with Refractive Index Detector for Quantification of Memantine Hydrochloride in Dissolution Samples.

PubMed

Sawant, Tukaram B; Wakchaure, Vikas S; Rakibe, Udyakumar K; Musmade, Prashant B; Chaudhari, Bhata R; Mane, Dhananjay V

2017-07-01

The present study was aimed to develop an analytical method for quantification of memantine (MEM) hydrochloride in dissolution samples using high-performance liquid chromatography with refractive index (RI) detector. The chromatographic separation was achieved on C18 (250 × 4.5 mm, 5 μm) column using isocratic mobile phase comprises of buffer (pH 5.2):methanol (40:60 v/v) pumped at a flow rate of 1.0 mL/min. The column effluents were monitored using RI detector. The retention time of MEM was found to be ~6.5 ± 0.3 min. The developed chromatographic method was validated and found to be linear over the concentration range of 5.0-45.0 μg/mL for MEM. Mean recovery of MEM was found to be 99.2 ± 0.5% (w/w). The method was found to be simple, fast, precise and accurate, which can be utilized for the quantification of MEM in dissolution samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Practical method for the definition of chromatographic peak parameters in preparative liquid chromatography.

PubMed

Jin, Gaowa; Guo, Zhimou; Xiao, Yuansheng; Yan, Jingyu; Dong, Xuefang; Shen, Aijin; Wang, Chaoran; Liang, Xinmiao

2016-10-01

A practical method was established for the definition of chromatographic parameters in preparative liquid chromatography. The parameters contained both the peak broadening level under different amounts of sample loading and the concentration distribution of the target compound in the elution. The parameters of the peak broadening level were defined and expressed as a matrix, which consisted of sample loading, the forward broadening and the backward broadening levels. The concentration distribution of the target compound was described by the heat map of the elution profile. The most suitable stationary phase should exhibit the narrower peak broadening and it was best to broaden to both sides to compare to the peak under analytical conditions. Besides, the concentration distribution of the target compounds should be focused on the middle of the elution. The guiding principles were validated by purification of amitriptyline from the mixture of desipramine and amitriptyline. On the selected column, when the content of the impurity desipramine was lower than 0.1%, the recovery of target compound was much higher than the other columns even when the sample loading was as high as 8.03 mg/cm 3 . The parameters and methods could be used for the evaluation and selection of stationary phases in preparative chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

PubMed

Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

2017-04-15

A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up].

PubMed

Zhang, Chunyu; Wang, Hui; Zhang, Xiaohui; Ma, Zhongqiang; Deng, Wanmei; Hu, Ke; Ding, Mingyu

2011-12-01

A method of gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) was established for the simultaneous determination of 5 main phthalate plasticizers in foods (edible oil, instant noodles, fried pastries, Saqima, etc.). The samples were extracted with petroleum ether in an ultrasonator, purified by a GPC column, and analyzed by HPLC. The chromatographic separation was achieved on a Labtech-C18 column (250 mm x 4.6 mm, 5 microm) using acetonitrile and water mixture as the mobile phases in a gradient elution mode. The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25 - 13.4 microg/L. The spike recoveries were between 70.4% and 113.6% with the relative standard deviations (RSDs, n = 3) of 0.3% - 5.8% at the spiked level of 50 mg/L. This method is simple, rapid and practical, and can be used for the simultaneous determination of PAEs in grease food samples.

Characterization of Chinese rice wine taste attributes using liquid chromatographic analysis, sensory evaluation, and an electronic tongue.

PubMed

Yu, HaiYan; Zhao, Jie; Li, Fenghua; Tian, Huaixiang; Ma, Xia

2015-08-01

To evaluate the taste characteristics of Chinese rice wine, wine samples sourced from different vintage years were analyzed using liquid chromatographic analysis, sensory evaluation, and an electronic tongue. Six organic acids and seventeen amino acids were measured using high performance liquid chromatography (HPLC). Five monosaccharides were measured using anion-exchange chromatography. The global taste attributes were analyzed using an electronic tongue (E-tongue). The correlations between the 28 taste-active compounds and the sensory attributes, and the correlations between the E-tongue response and the sensory attributes were established via partial least square discriminant analysis (PLSDA). E-tongue response data combined with linear discriminant analysis (LDA) were used to discriminate the Chinese rice wine samples sourced from different vintage years. Sensory evaluation indicated significant differences in the Chinese rice wine samples sourced from 2003, 2005, 2008, and 2010 vintage years in the sensory attributes of harmony and mellow. The PLSDA model for the taste-active compounds and the sensory attributes showed that proline, fucose, arabinose, lactic acid, glutamic acid, arginine, isoleucine, valine, threonine, and lysine had an influence on the taste characteristic of Chinese rice wine. The Chinese rice wine samples were all correctly classified using the E-tongue and LDA. The electronic tongue was an effective tool for rapid discrimination of Chinese rice wine. Copyright © 2015 Elsevier B.V. All rights reserved.

[Identification of impurity peaks in the HPLC chromatogram by LC-MS and two-dimensional chromatographic correlation spectroscopy].

PubMed

Chen, Zhen-Zhen; Zhang, Dou-Sheng; Wang, Nan; Feng, Fang; Hu, Chang-Qin

2012-04-01

A novel qualitative analytical method by using two-dimensional chromatographic correlation spectroscopy techniques for recognizing impurity peaks of HPLC methods of quality control and LC-MS chromatographic system was established. The structures of major degradation products of ceftizoxime and cefdinir were identified by LC-MS and MassWorks application; the standard chromatographic and spectral data of the degradation impurities were obtained by high-performance liquid chromatography with diode array detection. The impurity peaks of two-dimensional chromatography were matched by comparison of spectra and calculating correlation coefficients. Peaks in chromatography can be identified accurately and rapidly in different chromatographic systems such as column and mobile phase changed. The method provides a new way and thought to identify the peaks in quality control of impurities without reference impurity substances.

Multivariate curve-resolution analysis of pesticides in water samples from liquid chromatographic-diode array data.

PubMed

Maggio, Rubén M; Damiani, Patricia C; Olivieri, Alejandro C

2011-01-30

Liquid chromatographic-diode array detection data recorded for aqueous mixtures of 11 pesticides show the combined presence of strongly coeluting peaks, distortions in the time dimension between experimental runs, and the presence of potential interferents not modeled by the calibration phase in certain test samples. Due to the complexity of these phenomena, data were processed by a second-order multivariate algorithm based on multivariate curve resolution and alternating least-squares, which allows one to successfully model both the spectral and retention time behavior for all sample constituents. This led to the accurate quantitation of all analytes in a set of validation samples: aldicarb sulfoxide, oxamyl, aldicarb sulfone, methomyl, 3-hydroxy-carbofuran, aldicarb, propoxur, carbofuran, carbaryl, 1-naphthol and methiocarb. Limits of detection in the range 0.1-2 μg mL(-1) were obtained. Additionally, the second-order advantage for several analytes was achieved in samples containing several uncalibrated interferences. The limits of detection for all analytes were decreased by solid phase pre-concentration to values compatible to those officially recommended, i.e., in the order of 5 ng mL(-1). Copyright © 2010 Elsevier B.V. All rights reserved.

Liquid chromatographic determination of chloramine-T and its primary degradation product, p-toluenesulfonamide, in water

USGS Publications Warehouse

Dawson, Verdel K.; Davis, Ruth A.

1997-01-01

N-sodium-N-chloro-rho-toluenesulfonamide (chloramine-T) effectively controls bacterial gill disease (BGD) in cultured fishes, BGD, a common disease of hatchery-reared salmonids, causes more fish losses than any other disease among these species. This study describes a liquid chromatographic (LC) method that is capable of direct, simultaneous analysis of chloramine-T and its primary degradation product, rho-toluenesulfonamide (rho-TSA), in water. The procedure involves reversed-phase (C-18) LC analysis with ion suppression, using 0.01 M phosphate buffer at pH 3. The mobile phase is phosphate buffer-acetonitrile (60 + 40) at 1 mL/min. Both chemicals can be detected with a UV spectrophotometer at 229 nm; the method is linear up to 40 mg, chloramine-T or rho-TSA/L. Mean recoveries were 96.4 +/- 6.1% for water samples fortified with 0.03 mg chloramine-T/L and 95.3 +/- 4.6% for water samples fortified with 0.005 mg rho-TSA/L. Limits of detection without sample enrichment for chloramine-T and rho-TSA are 0.01 mg/L and 0.001 mg/L, respectively.

Liquid chromatographic determination of chloramine-T and its primary degradation product, p-toluenesulfonamide, in water

USGS Publications Warehouse

Dawson, V.K.; Davis, R.A.

1997-01-01

N-sodium-N-chloro-rho-toluenesulfonamide (chloramine-T) effectively controls bacterial gill disease (BGD) in cultured fishes, BGD, a common disease of hatchery-reared salmonids, causes more fish losses than any other disease among these species, This study describes a liquid chromatographic (LC) method that is capable of direct, simultaneous analysis of chloramine-T and its primary degradation product, rho-toluenesulfonamide (rho-TSA), in water. The procedure involves reversed-phase (C-18) LC analysis with ion suppression, using 0.01 M phosphate buffer at pH 3. The mobile phase is phosphate buffer-acetonitrile (60 + 40) at 1 mL/min. Both chemicals can be detected with a UV spectrophotometer at 229 nm; the method is linear up to 40 mg, chloramine-T or rho-TSA/L. Mean recoveries were 96.4 +/- 6.1% for water samples fortified with 0.03 mg chloramine-T/L and 95.3 +/- 4.6% for water samples fortified with 0.005 mg rho-TSA/L. Limits of detection without sample enrichment for chloramine-T and rho-TSA are 0.01 mg/L and 0.001 mg/L, respectively.

Exploiting the synergistic effect of concurrent data signals: Low-level fusion of liquid chromatographic with dual detection data.

PubMed

Teglia, Carla M; Azcarate, Silvana M; Alcaráz, Mirta R; Goicoechea, Héctor C; Culzoni, María J

2018-08-15

A low-level data fusion strategy was developed and implemented for data processing of second-order liquid chromatographic data with dual detection, i.e. absorbance and fluorescence monitoring. The synergistic effect of coupling individual information provided by two different detectors was evaluated by analyzing the results gathered after the application of a series of data preprocessing steps and chemometric resolution. The chemometric modeling involved data analysis by MCR-ALS, PARAFAC and N-PLS. Their ability to handle the new data block was assessed through the estimation of the analytical figures of merits achieved in the prediction of a validation set containing fifteen fluorescent and non-fluorescent veterinary active ingredients that can be found in poultry litter. Eventually, the feasibility of the application of the fusion strategy to real poultry litter samples containing the studied compounds was verified. Copyright © 2018 Elsevier B.V. All rights reserved.

Supercharging Reagent for Enhanced Liquid Chromatographic Separation and Charging of Sialylated and High-Molecular-Weight Glycopeptides for NanoHPLC-ESI-MS/MS Analysis.

PubMed

Lin, Chia-Wei; Haeuptle, Micha A; Aebi, Markus

2016-09-06

Recent developments in proteomic techniques have led to the development of mass spectrometry (MS)-based methods to characterize site-specific glycosylation of proteins. However, appropriate analytical tools to characterize acidic and high-molecular-weight (hMW) glycopeptides are still lacking. In this study, we demonstrate that the addition of supercharging reagent, m-nitrobenzyl alcohol (m-NBA), into mobile phases greatly facilitates the analysis of acidic and hMW glycopeptides. Using commercial glycoproteins, we demonstrated that in the presence of m-NBA the charge state of sialylated glycopeptides increased and the chromatographic separation of neutral and acidic glycopeptides revealed a remarkable improvement. Next, we applied this system to the characterization of a glycoconjugate vaccine candidate consisting of a genetically detoxified exotoxin A of Pseudomonas aeruginosa covalently linked to Shigella flexneri type 2a O-antigen (Sf2E) produced by engineered Escherichia coli. The addition of m-NBA, allowed us to identify peptides with glycan chains of unprecedented size, up to 20 repeat units (98 monosaccharides). Our results indicated that incorporation of m-NBA into reversed-phase liquid chromatography (LC) solvents improves sensitivity, charging, and chromatographic resolution for acidic and hMW glycopeptides.

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

PubMed

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

2014-12-29

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

Characterization of Coconut Oil Fractions Obtained from Solvent Fractionation Using Acetone.

PubMed

Sonwai, Sopark; Rungprasertphol, Poonyawee; Nantipipat, Nantinee; Tungvongcharoan, Satinee; Laiyangkoon, Nantikan

2017-09-01

This work was aimed to study the solvent fraction of coconut oil (CNO). The fatty acid and triacylglycerol compositions, solid fat content (SFC) and the crystallization properties of CNO and its solid and liquid fractions obtained from fractionation at different conditions were investigated using various techniques. CNO was dissolved in acetone (1:1 w/v) and left to crystallize isothermally at 10°C for 0.5, 1 and 2 h and at 12°C for 2, 3 and 6 h. The solid fractions contained significantly lower contents of saturated fatty acids of ≤ 10 carbon atoms but considerably higher contents of saturated fatty acids with > 12 carbon atoms with respect to those of CNO and the liquid fractions. They also contained higher contents of high-melting triacylglycerol species with carbon number ≥ 38. Because of this, the DSC crystallization onset temperatures and the crystallization peak temperatures of the solid fractions were higher than CNO and the liquid fractions. The SFC values of the solid fractions were significantly higher than CNO at all measuring temperatures before reaching 0% just below the body temperature with the fraction obtained at 12°C for 2 h exhibiting the highest SFC. On the contrary, the SFC values of the liquid fractions were lower than CNO. The crystallization duration exhibited strong influence on the solid fractions. There was no effect on the crystal polymorphic structure possibly because CNO has β'-2 as a stable polymorph. The enhanced SFC of the solid fractions would allow them to find use in food applications where a specific melting temperature is desired such as sophisticated confectionery fats, and the decreased SFC of the liquid fractions would provide them with a higher cold stability which would be useful during extended storage time.

Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology.

PubMed

Brown, Leslie; Earle, Martyn J; Gîlea, Manuela A; Plechkova, Natalia V; Seddon, Kenneth R

2017-08-10

Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous character of ionic liquid-based solvent systems to be used in a wide variety of separations (including transition metal salts, arenes, alkenes, alkanes, bio-oils and sugars).

Chromatographic fractionation and molecular mass characterization of Cercidium praecox (Brea) gum.

PubMed

Castel, Virginia; Zivanovic, Svetlana; Jurat-Fuentes, Juan L; Santiago, Liliana G; Rubiolo, Amelia C; Carrara, Carlos R; Harte, Federico M

2016-10-01

Brea gum (BG) is an exudate from the Cercidium praecox tree that grows in semi-arid regions of Argentina. Some previous studies on BG have shown physicochemical characteristics and functional features similar to those of gum arabic. However, there is a need to elucidate the molecular structure of BG to understand the functionality. In this sense, BG was fractionated using hydrophobic interaction chromatography and the obtained fractions were analyzed by size exclusion chromatography. Analysis of the fractions showed that the bulk of the gum (approx. 84% of the polysaccharides) was a polysaccharide of 2.79 × 10(3)  kDa. The second major fraction (approx. 16% of the polysaccharides) was a polysaccharide-protein complex with a molecular mass of 1.92 × 10(5)  kDa. A third fraction consisted of protein species with a wide range of molecular weights. The molecular weight distribution of the protein fraction was analyzed by size exclusion chromatography. Comparison of the elution profiles of the exudates in native and reducing conditions revealed that some of the proteins were forming aggregates through disulfide bridges in native conditions. Further analysis of the protein fraction by SDS-PAGE showed proteins with molecular weight ranging from 6.5 to 66 kDa. The findings showed that BG consists of several fractions with heterogeneous chemical composition and polydisperse molecular weight distributions. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Chromatographic instrumentation in space: past, present and future developments for exobiological studies

NASA Astrophysics Data System (ADS)

Raulin, F.; Sternberg, R.; Coscia, D.; Vidal-Madjar, C.; Millot, M.-C.; Sébille, B.; Israel, G.

1999-01-01

Several planetary exploration missions have already used chromatographic techniques to search for organic compounds, including complex organics, in extraterrestrial environments. So far, only gas chromatography (GC) has been used. In two cases (Viking and Cassini-Huygens), a Py-GC-MS instrument, coupling GC with a pyrolyzer and a mass spectrometer, has been flown. Powerful miniaturized Py-GC-MS instrumentation, with high resolution multi-GC columns and time-of-flight or Ion Trap mass spectrometers are under development, in the frame of the preparation of the Rosetta mission. There is now a strong need for new chromatographic instrumentation in space, in particular to perform detailed molecular analyses of complex non-volatile organics, including macromolecular compounds. Liquid Chromatography (LC), in particular High Performance Liquid Chromatography (HPLC) Supercritical Fluid Chromatography (SFC) or Chemical-Derivatization Gas Chromatography (CDGC) could provide a very efficient mean of analyzing a wide variety of exobiologically important compounds. LC or CDGC have never been used in space yet, but feasibility studies on their application in planetary mission are needed.

Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

PubMed

Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

2015-06-01

An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An improved high-performance liquid chromatographic method for simultaneous determination of tocopherols, tocotrienols and γ-oryzanol in rice.

PubMed

Huang, Shao-Hua; Ng, Lean-Teik

2011-07-22

An improved normal phase high performance liquid chromatographic (NP-HPLC) method was developed for simultaneous quantification of eight vitamin E isomers (α-, β-, γ- and δ-tocopherols and α-, β-, γ- and δ-tocotrienols) and γ-oryzanol in rice. A complete separation of all compounds was achieved within 25 min using an Inertsil CN-3, SIL-100A 5 μM (4.6 mm × 250 mm) column and an isocratic elution system of hexane/isopropanol/ethylacetate/acetic acid (97.6:0.8:0.8:0.8, v/v/v/v) at a flow rate varying from 0.7 to 1.5 mL min(-1). A linear correlation coefficient (r(2)>0.99) and high reproducibility were obtained at concentrations ranging 0.05-10 μg mL(-1) for vitamin E isomers and 0.5-500 μg mL(-1) for γ-oryzanol. This method proved to be rapid, accurate and reproducible. Copyright © 2011 Elsevier B.V. All rights reserved.

Chromatographic separation of radioactive noble gases from xenon

NASA Astrophysics Data System (ADS)

Akerib, D. S.; Araújo, H. M.; Bai, X.; Bailey, A. J.; Balajthy, J.; Beltrame, P.; Bernard, E. P.; Bernstein, A.; Biesiadzinski, T. P.; Boulton, E. M.; Bramante, R.; Cahn, S. B.; Carmona-Benitez, M. C.; Chan, C.; Chiller, A. A.; Chiller, C.; Coffey, T.; Currie, A.; Cutter, J. E.; Davison, T. J. R.; Dobi, A.; Dobson, J. E. Y.; Druszkiewicz, E.; Edwards, B. N.; Faham, C. H.; Fiorucci, S.; Gaitskell, R. J.; Gehman, V. M.; Ghag, C.; Gibson, K. R.; Gilchriese, M. G. D.; Hall, C. R.; Hanhardt, M.; Haselschwardt, S. J.; Hertel, S. A.; Hogan, D. P.; Horn, M.; Huang, D. Q.; Ignarra, C. M.; Ihm, M.; Jacobsen, R. G.; Ji, W.; Kamdin, K.; Kazkaz, K.; Khaitan, D.; Knoche, R.; Larsen, N. A.; Lee, C.; Lenardo, B. G.; Lesko, K. T.; Lindote, A.; Lopes, M. I.; Manalaysay, A.; Mannino, R. L.; Marzioni, M. F.; McKinsey, D. N.; Mei, D.-M.; Mock, J.; Moongweluwan, M.; Morad, J. A.; Murphy, A. St. J.; Nehrkorn, C.; Nelson, H. N.; Neves, F.; O'Sullivan, K.; Oliver-Mallory, K. C.; Palladino, K. J.; Pease, E. K.; Pech, K.; Phelps, P.; Reichhart, L.; Rhyne, C.; Shaw, S.; Shutt, T. A.; Silva, C.; Solovov, V. N.; Sorensen, P.; Stephenson, S.; Sumner, T. J.; Szydagis, M.; Taylor, D. J.; Taylor, W.; Tennyson, B. P.; Terman, P. A.; Tiedt, D. R.; To, W. H.; Tripathi, M.; Tvrznikova, L.; Uvarov, S.; Verbus, J. R.; Webb, R. C.; White, J. T.; Whitis, T. J.; Witherell, M. S.; Wolfs, F. L. H.; Yazdani, K.; Young, S. K.; Zhang, C.

2018-01-01

The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes 85Kr and 39Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search experiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

Chromatographic separation of radioactive noble gases from xenon

DOE PAGES

Akerib, DS; Araújo, HM; Bai, X; ...

2017-10-31

The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopesmore » $$^{85}$$Kr and $$^{39}$$Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search exmperiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.« less

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

PubMed

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.

New acyclic secondary metabolites from the biologically active fraction of Albizia lebbeck flowers.

PubMed

Al-Massarani, Shaza M; El Gamal, Ali A; Abd El Halim, Mohamed F; Al-Said, Mansour S; Abdel-Kader, Maged S; Basudan, Omer A; Alqasoumi, Saleh I

2017-01-01

The total extract of Albizia lebbeck flowers was examined in vivo for its possible hepatoprotective activity in comparison with the standard drug silymarin at two doses. The higher dose expressed promising activity especially in reducing the levels of AST, ALT and bilirubin. Fractionation via liquid-liquid partition and reexamination of the fractions revealed that the n -butanol fraction was the best in improving liver biochemical parameters followed by the n -hexane fraction. However, serum lipid parameters were best improved with CHCl 3 fraction. The promising biological activity results initiated an intensive chromatographic purification of A. lebbeck flowers fractions. Two compounds were identified from natural source for the first time, the acyclic farnesyl sesquiterpene glycoside1-O-[6-O- α -l-arabinopyranosyl- β -d-glucopyranoside]-(2 E ,6 E -)-farnesol ( 6 ) and the squalene derivative 2,3-dihydroxy-2,3-dihydrosqualene ( 9 ), in addition to eight compounds reported here for the first time from the genus Albizia ; two benzyl glycosides, benzyl 1-O- β -d-glucopyranoside ( 1 ) and benzyl 6-O- α -l-arabinopyranosyl β -d-glucopyranoside ( 2 ); three acyclic monoterpene glycosides, linalyl β -d-glucopyranoside ( 3 ) and linalyl 6-O- α -l-arabinopyranosyl- β -d-glucopyranoside ( 4 ); (2 E )-3,7-dimethylocta-2,6-dienoate-6-O- α -l arabinopyranosyl- β -d-glucopyranoside ( 5 ), two oligoglycosides, n -hexyl- α -l arabinopyranosyl-(1 → 6)- β -d-glucopyranoside (creoside) ( 7 ) and n -octyl α -l-arabinopyranosyl-(1 → 6)- β -d-glucopyranoside (rhodiooctanoside) ( 8 ); and ethyl fructofuranoside ( 10 ). The structures of the isolated compounds were elucidated based on extensive examination of their spectroscopic 1D and 2D-NMR, MS, UV, and IR data. It is worth mentioning that, some of the isolated linalol glycoside derivatives were reported as aroma precursors.

Experimental determination of the Mo isotope fractionation factor between metal and silicate liquids

NASA Astrophysics Data System (ADS)

Hin, R. C.; Burkhardt, C.; Schmidt, M. W.; Bourdon, B.

2011-12-01

The conditions and chemical consequences of core formation have mainly been reconstructed from experimentally determined element partition coefficients between metal and silicate liquids. However, first order questions such as the mode of core formation or the nature of the light element(s) in the Earth's core are still debated [1]. In addition, the geocentric design of most experimental studies leaves the conditions of core formation on other terrestrial planets and asteroids even more uncertain than for Earth. Through mass spectrometry, records of mass-dependent stable isotope fractionation during high-temperature processes such as metal-silicate segregation are detectable. Stable isotope fractionation may thus yield additional constrains on core formation conditions and its consequences for the chemical evolution of planetary objects. Experimental investigations of equilibrium mass-dependent stable isotope fractionation have shown that Si isotopes fractionate between metal and silicate liquids at temperatures of 1800°C and pressures of 1 GPa, while Fe isotopes leave no resolvable traces of core formation processes [2,3]. Molybdenum is a refractory and siderophile trace element in the Earth, and thus much less prone to complications arising from mass balancing core and mantle and from potential volatile behaviour than other elements. To determine equilibrium mass-dependent Mo isotope fractionation during metal-silicate segregation, we have designed piston cylinder experiments with a basaltic silicate composition and an iron based metal with ~8 wt% Mo, using both graphite and MgO capsules. Metal and silicate phases are completely segregated by the use of a centrifuging piston cylinder at ETH Zurich, thus preventing analysis of mixed metal and silicate signatures. Molybdenum isotope compositions were measured using a Nu Instruments 1700 MC-ICP-MS at ETH Zurich. To ensure an accurate correction of analytical mass fractionation a 100Mo-97Mo double spike was admixed

Liquid chromatographic determination of oxytetracycline in edible fish fillets from six species of fish

USGS Publications Warehouse

Meinertz, J.R.; Stehly, G.R.; Gingerich, W.H.

1998-01-01

The approved use of oxytetracycline (OTC) in U.S. Aquaculture is limited to specific diseases in salmonids and channel catfish. OTC may also be effective in controlling diseases in other fish species important to public aquaculture, but before approved use of OTC can be augmented, an analytical method for determining OTC in fillet tissue from multiple species of fish will be required to support residue depletion studies. The objective of this study was to develop and validate a liquid chromatographic (LC) method that is accurate, precise, and sensitive for OTC in edible fillets from multiple species of fish. Homogenized fillet tissues from walleye, Atlantic salmon, striped bass, white sturgeon, rainbow trout, and channel catfish were fortified with OTC at nominal concentrations of 10, 20, 100, 1000, and 5000 ng/g. In tissues fortified with OTC at 100, 1000, and 5000 ng/g, mean recoveries ranged from 83 to 90%, and relative standard deviations (RSDs) ranged from 0.9 to 5.8%. In all other tissues, mean recoveries ranged from 59 to 98%, and RSDs ranged from 3.3 to 20%. Method quantitation limits ranged from 6 to 22 ng/g for the 6 species. The LC parameters produced easily integratable OTC peaks without coelution of endogenous compounds. The method is accurate, precise, and sensitive for OTC in fillet tissue from 6 species of fish from 5 phylogenetically diverse groups.

Chromatographic performance of synthetic polycrystalline diamond as a stationary phase in normal phase high performance liquid chromatography.

PubMed

Peristyy, Anton; Paull, Brett; Nesterenko, Pavel N

2015-04-24

The chromatographic properties of high pressure high temperature synthesised diamond (HPHT) are investigated in normal phase mode of high performance liquid chromatography. Purified nonporous irregular shape particles of average particles size 1.2 μm and specific surface area 5.1 m(2) g(-1) were used for packing 100×4.6 mm ID or 50×4.6 mm ID stainless steel columns. The retention behaviour of several classes of compounds including alkyl benzenes, polyaromatic hydrocarbons (PAH), alkylphenylketones, phenols, aromatic acids and bases were studied using n-hexane-2-propanol mixtures as mobile phase. The results are compared with those observed for microdispersed sintered detonation nanodiamond (MSDN) and porous graphitic carbon (PGC). HPHT diamond revealed distinctive separation selectivity, which is orthogonal to that observed for porous graphitic carbon; while selectivities of HPHT diamond and microdispersed sintered detonation nanodiamonds are similar. Owing to non-porous particle nature, columns packed with high pressure high temperature diamond exhibited excellent mass transfer and produce separations with maximum column efficiency of 128,200 theoretical plates per meter. Copyright © 2015 Elsevier B.V. All rights reserved.

Liquid chromatographic separation and thermodynamic investigation of lorcaserin hydrochloride enantiomers on immobilized amylose-based chiral stationary phase.

PubMed

Wani, Dattatraya V; Rane, Vipul P; Mokale, Santosh N

2018-03-01

A novel liquid chromatographic method was developed for enantiomeric separation of lorcaserin hydrochloride on Chiralpak IA column containing chiral stationary phase immobilized with amylose tris (3.5-dimethylphenylcarbamate) as chiral selector. Baseline separation with resolution greater than 4 was achieved using mobile phase containing mixture of n-hexane/ethanol/methanol/diethylamine (95:2.5:2.5:0.1, v/v/v/v) at a flow rate of 1.2 mL/min. The limit of detection and limit of quantification of the S-enantiomer were found to be 0.45 and 1.5 μg/mL, respectively; the developed method was validated as per ICH guideline. The influence of column oven temperatures studied in the range of 20°C to 50°C on separation was studied; from this, retention, separation, and resolution were investigated. The thermodynamic parameters ΔH°, ΔS°, and ΔG° were evaluated from van't Hoff plots,(Ink' versus 1/T) and used to explain the strength of interaction between enantiomers and immobilized amylose-based chiral stationary phase. © 2017 Wiley Periodicals, Inc.

[Effects of carrier liquid and flow rate on the separation in gravitational field-flow fractionation].

PubMed

Guo, Shuang; Zhu, Chenqi; Gao-Yang, Yaya; Qiu, Bailing; Wu, Di; Liang, Qihui; He, Jiayuan; Han, Nanyin

2016-02-01

Gravitational field-flow fractionation is the simplest field-flow fractionation technique in terms of principle and operation. The earth' s gravity is its external field. Different sized particles are injected into a thin channel and carried by carrier fluid. The different velocities of the carrier liquid in different places results in a size-based separation. A gravitational field-flow fractionation (GrFFF) instrument was designed and constructed. Two kinds of polystyrene (PS) particles with different sizes (20 µm and 6 µm) were chosen as model particles. In this work, the separation of the sample was achieved by changing the concentration of NaN3, the percentage of mixed surfactant in the carrier liquid and the flow rate of carrier liquid. Six levels were set for each factor. The effects of these three factors on the retention ratio (R) and plate height (H) of the PS particles were investigated. It was found that R increased and H decreased with increasing particle size. On the other hand, the R and H increased with increasing flow rate. The R and H also increased with increasing NaN3 concentration. The reason was that the electrostatic repulsive force between the particles and the glass channel wall increased. The force allowed the samples approach closer to the channel wall. The results showed that the resolution and retention time can be improved by adjusting the experimental conditions. These results can provide important values to the further applications of GrFFF technique.

Chromatographic Separations Using Solid-Phase Extraction Cartridges: Separation of Wine Phenolics

NASA Astrophysics Data System (ADS)

Brenneman, Charles A.; Ebeler, Susan E.

1999-12-01

We describe a simple laboratory experiment that demonstrates the principles of chromatographic separation using solid-phase extraction columns and red wine. By adjusting pH and mobile phase composition, the wine is separated into three fractions of differing polarity. The content of each fraction can be monitored by UV-vis spectroscopy. When the experiment is combined with experiments involving HPLC or GC separations, students gain a greater appreciation for and understanding of the highly automated instrumental systems currently available. In addition, they learn about the chemistry of polyphenolic compounds, which are present in many foods and beverages and which are receiving much attention for their potentially beneficial health effects.

Identification of intact high molecular weight glutenin subunits from the wheat proteome using combined liquid chromatography-electrospray ionization mass spectrometry.

PubMed

Lagrain, Bert; Brunnbauer, Markus; Rombouts, Ine; Koehler, Peter

2013-01-01

The present paper describes a method for the identification of intact high molecular weight glutenin subunits (HMW-GS), the quality determining proteins from the wheat storage proteome. The method includes isolation of HMW-GS from wheat flour, further separation of HMW-GS by reversed-phase high-performance liquid chromatography (RP-HPLC), and their subsequent molecular identification with electrospray ionization mass spectrometry using a quadrupole-time-of-flight mass analyzer. For HMW-GS isolation, wheat proteins were reduced and extracted from flour with 50% 1-propanol containing 1% dithiothreitol. HMW-GS were then selectively precipitated from the protein mixture by adjusting the 1-propanol concentration to 60%. The composition of the precipitated proteins was first evaluated by sodium dodecyl sulfate-polyacrylamide gel electrophoresis with Coomassie staining and RP-HPLC with ultraviolet detection. Besides HMW-GS (≥65%), the isolated proteins mainly contained ω5-gliadins. Secondly, the isolated protein fraction was analyzed by liquid chromatography-mass spectrometry. Optimal chromatographic separation of HMW-GS from the other proteins in the isolated fraction was obtained when the mobile phase contained 0.1% trifluoroacetic acid as ion-pairing agent. Individual HMW-GS were then identified by determining their molecular masses from the high-resolution mass spectra and comparing these with theoretical masses calculated from amino acid sequences. Using formic acid instead of trifluoroacetic acid in the mobile phase increased protein peak intensities in the base peak mass chromatogram. This allowed the detection of even traces of other wheat proteins than HMW-GS in the isolated fraction, but the chromatographic separation was inferior with a major overlap between the elution ranges of HMW-GS and ω-gliadins. Overall, the described method allows a rapid assessment of wheat quality through the direct determination of the HMW-GS composition and offers a basis for

Lipophilicity indices derived from the liquid chromatographic behavior observed under bimodal retention conditions (reversed phase/hydrophilic interaction): application to a representative set of pyridinium oximes.

PubMed

Voicu, Victor; Sârbu, Costel; Tache, Florentin; Micăle, Florina; Rădulescu, Ştefan Flavian; Sakurada, Koichi; Ohta, Hikoto; Medvedovici, Andrei

2014-05-01

The liquid chromatographic behavior observed under bimodal retention conditions (reversed phase and hydrophilic interaction) offers a new basis for the determination of some derived lipophilicity indices. The experiments were carried out on a representative group (30 compounds) of pyridinium oximes, therapeutically tested in acetylcholinesterase reactivation, covering a large range of lipophilic character. The chromatographic behavior was observed on a mixed mode acting stationary phase, resulting from covalent functionalization of high purity spherical silica with long chain alkyl groups terminated by a polar environment created through the vicinal diol substitution at the lasting carbon atoms (Acclaim Mixed Mode HILIC 1 column). Elution was achieved by combining different proportions of 5 mM ammonium formiate solutions in water and acetonitrile. The derived lipophilicity indices were compared with logP values resulting from different computational algorithms. The correlations between experimental and computed data sets are significant. To obtain a better insight on the transition from reversed phase to hydrophilic interaction retention mechanisms, the variation of the thermodynamic parameters determined through the van׳t Hoff approach was also discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Use of high pressure liquid chromatography in the study of liquid lubricant oxidation

NASA Technical Reports Server (NTRS)

Morales, W.

1982-01-01

The general principles of classical liquid chromatography and high-pressure liquid chromatography (HPLC) are reviewed, and their advantages and disadvantages are compared. Several chromatographic techniques are reviewed, and the analysis of a C-ether liquid lubricant by each technique is illustrated. An analysis by size exclusion chromatography of an ester lubricant, which had been degraded using a micro-oxidation apparatus, is illustrated to show how HPLC can be used in the study of high-temperature lubricant degradation.

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

NASA Astrophysics Data System (ADS)

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

1989-09-01

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

Sheath liquid interface for the coupling of normal-phase liquid chromatography with electrospray mass spectrometry and its application to the analysis of neoflavonoids.

PubMed

Charles, Laurence; Laure, Frédéric; Raharivelomanana, Phila; Bianchini, Jean-Pierre

2005-01-01

A novel interface that allows normal-phase liquid chromatography to be coupled with electrospray ionization (ESI) is reported. A make-up solution of 60 mM ammonium acetate in methanol, infused at a 5 microl min(-1) flow-rate at the tip of the electrospray probe, provides a sheath liquid which is poorly miscible with the chromatographic effluent, but promotes efficient ionization of the targeted analytes. Protonated molecules generated in the ESI source were subjected to tandem mass spectrometric experiments in a triple-quadrupole mass spectrometer. The main fragmentation reactions were characterized for each analyte and specific mass spectral transitions were used to acquire chromatographic data in the multiple reaction monitoring detection mode. Results obtained during optimization of the sheath liquid composition and flow-rate suggest that the electrospray process was mainly under the control of the make-up solution, and that it forms an external charged layer around a neutral chromatographic mobile phase core. This sheath liquid interface was implemented for the analysis of some neoflavonoid compounds and its performance was evaluated. Limits of detection were established for calophillolide, inophyllum B, inophyllum P and inophyllum C at 100, 25, 15 and 100 ng ml(-1), respectively.

pH-dependence of single-protein adsorption and diffusion at a liquid chromatographic interface.

PubMed

Kisley, Lydia; Poongavanam, Mohan-Vivekanandan; Kourentzi, Katerina; Willson, Richard C; Landes, Christy F

2016-02-01

pH is a common mobile phase variable used to control protein separations due to the tunable nature of amino acid and adsorbent charge. Like other column variables such as column density and ligand loading density, pH is usually optimized empirically. Single-molecule spectroscopy extracts molecular-scale data to provide a framework for mechanistic optimization of pH. The adsorption and diffusion of a model globular protein, α-lactalbumin, was studied by single-molecule microscopy at a silica-aqueous interface analogous to aqueous normal phase and hydrophilic interaction chromatography and capillary electrophoresis interfaces at varied pH. Electrostatic repulsion resulting in free diffusion was observed at pH above the isoelectric point of the protein. In contrast, at low pH strong adsorption and surface diffusion with either no (D ∼ 0.01 μm(2) /s) or translational (D ∼ 0.3 μm(2) /s) motion was observed where the protein likely interacted with the surface through electrostatic, hydrophobic, and hydrogen bonding forces. The fraction of proteins immobilized could be increased by lowering the pH. These results show that retention of proteins at the silica interface cannot be viewed solely as an adsorption/desorption process and that the type of surface diffusion, which ultimately leads to ensemble chromatographic separations, can be controlled by tuning long-range electrostatic and short-range hydrophobic and hydrogen bonding forces with pH. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2013-08-09

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

Preparative isolation of flavonoid glycosides from Sphaerophysa salsula using hydrophilic interaction solid-phase extraction coupled with two-dimensional preparative liquid chromatography.

PubMed

Jiao, Lijin; Tao, Yanduo; Wang, Weidong; Shao, Yun; Mei, Lijuan; Wang, Qilan; Dang, Jun

2017-10-01

An offline preparative two-dimensional reversed-phase liquid chromatography/hydrophilic interaction liquid chromatography coupled with hydrophilic interaction solid-phase extraction method was developed for the preparative isolation of flavonoid glycosides from a crude sample of Sphaerophysa salsula. First, the non-flavonoids were removed using an XAmide solid-phase extraction cartridge. Based on the separation results of three different chromatographic stationary phases, the first-dimensional preparation was performed on an XAqua C18 prep column, and 15 fractions were obtained from the 5.2 g target sample. Then, three representative fractions were selected for additional purification on an XAmide preparative column to further isolate the flavonoid glycosides. In all, eight flavonoid glycosides were isolated in purities over 97%. The results demonstrated that the two-dimensional liquid chromatography method used in this study was effective for the preparative separation of flavonoid glycosides from Sphaerophysa salsula. Additionally, this method showed great potential for the separation of flavonoid glycosides from other plant materials. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In vitro anthelmintic effects of Spigelia anthelmia protein fractions against Haemonchus contortus.

PubMed

Araújo, Sandra Alves; Soares, Alexandra Martins Dos Santos; Silva, Carolina Rocha; Almeida Júnior, Eduardo Bezerra; Rocha, Cláudia Quintino; Ferreira, André Teixeira da Silva; Perales, Jonas; Costa-Júnior, Livio M

2017-01-01

Gastrointestinal nematodes are a significant concern for animal health and well-being, and anthelmintic treatment is mainly performed through the use of chemical products. However, bioactive compounds produced by plants have shown promise for development as novel anthelmintics. The aim of this study is to assess the anthelmintic activity of protein fractions from Spigelia anthelmia on the gastrointestinal nematode Haemonchus contortus. Plant parts were separated into leaves, stems and roots, washed with distilled water, freeze-dried and ground into a fine powder. Protein extraction was performed with sodium phosphate buffer (75 mM, pH 7.0). The extract was fractionated using ammonium sulfate (0-90%) and extensively dialyzed. The resulting fractions were named LPF (leaf protein fraction), SPF (stem protein fraction) and RPF (root protein fraction), and the protein contents and activities of the fractions were analyzed. H. contortus egg hatching (EHA), larval exsheathment inhibition (LEIA) and larval migration inhibition (LMIA) assays were performed. Proteomic analysis was conducted, and high-performance liquid chromatography (HPLC) chromatographic profiles of the fractions were established to identify proteins and possible secondary metabolites. S. anthelmia fractions inhibited H. contortus egg hatching, with LPF having the most potent effects (EC50 0.17 mg mL-1). During LEIA, SPF presented greater efficiency than the other fractions (EC50 0.25 mg mL-1). According to LMIA, the fractions from roots, stems and leaves also reduced the number of larvae, with EC50 values of 0.11, 0.14 and 0.21 mg mL-1, respectively. Protein analysis indicated the presence of plant defense proteins in the S. anthelmia fractions, including protease, protease inhibitor, chitinase and others. Conversely, secondary metabolites were absent in the S. anthemia fractions. These results suggest that S. anthelmia proteins are promising for the control of the gastrointestinal nematode H. contortus.

Silver-modified mobile phase for normal-phase liquid chromatographic determination of prostaglandins and their 5,6-trans isomers in prostaglandin bulk drugs and triacetin solutions.

PubMed

Kissinger, L D; Robins, R H

1985-03-15

A silver-modified, normal-phase, high-performance liquid chromatographic system has been developed for prostaglanding bulk drugs and triacetin solutions. Silver nitrate present in the mobile phase results in high selectivity for cis/trans isomers with conventional silica columns. Prostaglandins were esterified with alpha-bromo-2'-acetonaphthone prior to chromatography to provide high detectability at 254 nm. For dilute triacetin solutions, a sample preparation scheme based on gravity-flow chromatography with silica columns was developed to isolate the prostaglandin from triacetin prior to derivatization. The analytical technique was applied to triacetin solutions containing as little as 10 micrograms/ml arbaprostil [15-(R)-methyl-PGE2].

Hand-portable liquid chromatographic instrumentation.

PubMed

Sharma, Sonika; Tolley, Luke T; Tolley, H Dennis; Plistil, Alex; Stearns, Stanley D; Lee, Milton L

2015-11-20

Over the last four decades, liquid chromatography (LC) has experienced an evolution to smaller columns and particles, new stationary phases and low flow rate instrumentation. However, the development of person-portable LC has not followed, mainly due to difficulties encountered in miniaturizing pumps and detectors, and in reducing solvent consumption. The recent introduction of small, non-splitting pumping systems and UV-absorption detectors for use with capillary columns has finally provided miniaturized instrumentation suitable for high-performance hand-portable LC. Fully integrated microfabricated LC still remains a significant challenge. Ion chromatography (IC) has been successfully miniaturized and applied for field analysis; however, applications are mostly limited to inorganic and small organic ions. This review covers advancements that make possible more rapid expansion of portable forms of LC and IC. Copyright © 2015 Elsevier B.V. All rights reserved.

Quality assessment of Herba Leonuri based on the analysis of multiple components using normal- and reversed-phase chromatographic methods.

PubMed

Dong, Shuya; He, Jiao; Hou, Huiping; Shuai, Yaping; Wang, Qi; Yang, Wenling; Sun, Zheng; Li, Qing; Bi, Kaishun; Liu, Ran

2017-12-01

A novel, improved, and comprehensive method for quality evaluation and discrimination of Herba Leonuri has been developed and validated based on normal- and reversed-phase chromatographic methods. To identify Herba Leonuri, normal- and reversed-phase high-performance thin-layer chromatography fingerprints were obtained by comparing the colors and R f values of the bands, and reversed-phase high-performance liquid chromatography fingerprints were obtained by using an Agilent Poroshell 120 SB-C18 within 28 min. By similarity analysis and hierarchical clustering analysis, we show that there are similar chromatographic patterns in Herba Leonuri samples, but significant differences in counterfeits and variants. To quantify the bio-active components of Herba Leonuri, reversed-phase high-performance liquid chromatography was performed to analyze syringate, leonurine, quercetin-3-O-robiniaglycoside, hyperoside, rutin, isoquercitrin, wogonin, and genkwanin simultaneously by single standard to determine multi-components method with rutin as internal standard. Meanwhile, normal-phase high-performance liquid chromatography was performed by using an Agilent ZORBAX HILIC Plus within 6 min to determine trigonelline and stachydrine using trigonelline as internal standard. Innovatively, among these compounds, bio-active components of quercetin-3-O-robiniaglycoside and trigonelline were first determined in Herba Leonuri. In general, the method integrating multi-chromatographic analyses offered an efficient way for the standardization and identification of Herba Leonuri. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultra-performance liquid chromatographic determination of L-ergothioneine in commercially available classes of cow milk.

PubMed

Sotgia, Salvatore; Pisanu, Elisabetta; Cambedda, Debora; Pintus, Gianfranco; Carru, Ciriaco; Zinellu, Angelo

2014-09-01

A new efficient and sensitive precolumn hydrophilic interaction ultra-performance liquid chromatography (HILIC-UPLC) method was established for the quantitative determination of L-ergothioneine (ERT) in milk. After derivatization of ERT with 7-diethylamino-3-[4-(iodoacetamido)phenyl]-4-methylcoumarin, chromatographic separation was achieved in a fairly short time, less than 5 min, on a 100 × 2.1 mm Waters Cortecs UPLC HILIC 1.6-μm column, by using a mixture of 30 mmol/L ammonium acetate/acetonitrile (10:90, v/v) as a mobile phase flowing isocratically at 0.9 mL/min. Limit of detection and the limit of quantification were 0.03 and 0.10 μmol/L, respectively. The method exhibited linearity in a concentration range of 0.16 and 5.08 μmol/L. Mean recovery was 106.66%, whereas intra- and interassay precisions were determined to be within 6 RSD%. On average, ERT concentration in different commercially available classes of cow milk was found to be 0.442 ± 0.191 μmol/L, with the highest levels in the ultra-high temperature milks and low values in the unprocessed and HTST whole milks. In this light, our experiments suggest that ERT could be used as a marker for the heat treatment of milk. © 2014 Institute of Food Technologists®

Advantages of Data Fusion: First Multivariate Curve Resolution Analysis of Fused Liquid Chromatographic Second-Order Data with Dual Diode Array-Fluorescent Detection.

PubMed

Pellegrino Vidal, Rocío B; Ibañez, Gabriela A; Escandar, Graciela M

2017-03-07

For the first time, liquid chromatography-diode array detection (LC-DAD) and liquid-chromatography fluorescence detection (LC-FLD) second-order data, collected in a single chromatographic run, were fused and chemometrically processed for the quantitation of coeluting analytes. Two different experimental mixtures composed of fluorescent and nonfluorescent endocrine disruptors were analyzed. Adequate pretreatment of the matrices before their fusion was crucial to attain reliable results. Multivariate curve resolution-alternating least-squares (MCR-ALS) was applied to LC-DAD, LC-FLD, and fused LC-DAD-FLD data. Although different degrees of improvement are observed when comparing the fused matrix results in relation to those obtained using a single detector, clear benefits of data fusion are demonstrated through: (1) the obtained limits of detection in the ranges 2.1-24 ng mL -1 and 0.9-6.3 ng mL -1 for the two evaluated systems and (2) the low relative prediction errors, below 7% in all cases, indicating good recoveries and precision. The feasibility of fusing data and its advantages in the analysis of real samples was successfully assessed through the study of spiked tap, underground, and river water samples.

Isocratic non-aqueous reversed-phase high-performance liquid chromatographic separation of capsanthin and capsorubin in red peppers (Capsicum annuum L.), paprika and oleoresin.

PubMed

Weissenberg, M; Schaeffler, I; Menagem, E; Barzilai, M; Levy, A

1997-01-03

A simple, rapid high-performance liquid chromatography method has been devised in order to separate and quantify the xanthophylls capsorubin and capasanthin present in red pepper (Capsicum annuum L.) fruits and preparations made from them (paprika and oleoresin). A reversed-phase isocratic non-aqueous system allows the separation of xanthophylls within a few minutes, with detection at 450 nm, using methyl red as internal standard to locate the various carotenoids and xanthophylls found in plant extracts. The selection of extraction solvents, mild saponification conditions, and chromatographic features is evaluated and discussed. The method is proposed for rapid screening of large plant populations, plant selection, as well as for paprika products and oleoresin, and also for nutrition and quality control studies.

Storage temperature affects distribution of carbon, VFA, ammonia, phosphorus, copper and zinc in raw pig slurry and its separated liquid fraction.

PubMed

Popovic, Olga; Jensen, Lars Stoumann

2012-08-01

Chemical-mechanical separation of pig slurry into a solid fraction rich in dry matter, P, Cu and Zn and a liquid fraction rich in inorganic N but poor in dry matter may allow farmers to manage surplus slurry by exporting the solid fraction to regions with no nutrient surplus. Pig slurry can be applied to arable land only in certain periods during the year, so it is commonly stored prior to field application. This study investigated the effect of storage duration and temperature on chemical characteristics and P, Cu and Zn distribution between particle size classes of raw slurry and its liquid separation fraction. Dry matter, VFA, total N and ammonium content of both slurry products decreased during storage and were affected by temperature, showing higher losses at higher storage temperatures. In both products, total P, Cu and Zn concentrations were not significantly affected by storage duration or temperature. Particle size distribution was affected by slurry separation, storage duration and temperature. In raw slurry, particles larger than 1 mm decreased, whereas particles 250 μm-1 mm increased. The liquid fraction produced was free of particles >500 μm, with the highest proportions of P, Cu and Zn in the smallest particle size class (<25 μm). The proportion of particles <25 μm increased when the liquid fraction was stored at 5 °C, but decreased at 25 °C. Regardless of temperature, distribution of P, Cu and Zn over particle size classes followed a similar pattern to dry matter. Copyright © 2012 Elsevier Ltd. All rights reserved.

Optimization of chromatographic conditions for determination of aflatoxin B1, B2, G1 and G2 by using liquid chromatography-mass Spectrometry

NASA Astrophysics Data System (ADS)

Ramadhaningtyas, Dillani Putri; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

2017-11-01

The optimization of instrument condition and chromatographic separation for analysis of aflatoxin B1, B2, G1 and G2 using liquid chromatography tandem with mass spectrometer detector was conducted in the aim to provide more accurate and reliable analysis results. The aflatoxin known to be serious threat for human health as it is classified as the carcinogenic compounds. The aflatoxin B1, B2, G1 and G2 were selected due to its extensive contamination in various agricultural commodities. The best chromatographic separation was obtained using C-18 column with gradient elution of solvent 5 mM ammonium acetate and 0.1% formic acid in methanol at 7 minutes runtime analysis. The linearity of the detector showed satisfied results as the coefficient determination found to be 0.9994, 0.9996, 0.9998 and 0.9987 for aflatoxin B1, G1, B2, and G2 respectively in the range concentration from 1 to 20 ng/g. The quantifier ion selected for the aflatoxin B1, B2, G1 and G2 was m/z 285.1, 259, 243 and 313 respectively. The instrument precision at these quantifier ions also showed satisfied result with %RSD was around 3.4 to 6.8%. The optimized method present in this study can be used for further sample analysis.

Recent development of ionic liquid stationary phases for liquid chromatography.

PubMed

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.

Hydrocarbon Fuel Thermal Performance Modeling based on Systematic Measurement and Comprehensive Chromatographic Analysis

DTIC Science & Technology

2016-07-31

fueled liquid rocket engine, enthalpy is removed from the combustion chamber by a regenerative cooling system comprising a series of passages through... rocket engine, enthalpy is removed from the combustion chamber by a regenerative cooling system comprising a series of passages through which fuel flows...the unprecedented correlation of comprehensive two-dimensional gas chromatographic (GC×GC) rocket fuel data with physical and thermochemical

Identification of kinetin and kinetin riboside in coconut (Cocos nucifera L.) water using a combined approach of liquid chromatography-tandem mass spectrometry, high performance liquid chromatography and capillary electrophoresis.

PubMed

Ge, Liya; Yong, Jean Wan Hong; Goh, Ngoh Khang; Chia, Lian Sai; Tan, Swee Ngin; Ong, Eng Shi

2005-12-27

Kinetin (free base and riboside), which was assumed by many scientists to be a synthetic cytokinin plant growth hormone, has been detected for the first time in the endosperm liquid of fresh young coconut fruits ("coconut water"). To facilitate the study, we developed a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the identification and quantification of kinetin and kinetin riboside in purified coconut water extract sample. Following a solid-phase extraction of cytokinins in coconut water using C18 columns, the samples were further purified by Oasis MCX columns and analyzed by LC-MS/MS for kinetin and kinetin riboside. Detection by mass spectrometry was carried out using selected reaction monitoring (SRM) mode, by identifying the putative kinetin and kinetin riboside based on their characteristic fragments. Based on a signal-to-noise ratio of 3, the limits of detection in SRM mode were 0.02 microM and 0.005 microM for kinetin and kinetin riboside, respectively. Furthermore, optimal conditions for a baseline chromatographic separation of 18 cytokinin standards by high performance liquid chromatography (HPLC) were developed. The HPLC method had been employed for the confirmation and further fractionation of kinetin in coconut water extracts. The confirmation and fractionation of kinetin riboside was carried out using a further modified HPLC program due to the presence of other interfering material(s) in the sample matrix. Finally, fractions of putative kinetin and kinetin riboside collected from HPLC eluate of coconut water sample were further authenticated by independent capillary zone electrophoresis (CZE) experiment.

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

PubMed

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.

Fractional Brownian motion of an Al nanosphere in liquid Al-Si alloy under electron-beam irradiation

NASA Astrophysics Data System (ADS)

Yokota, Takeshi; Howe, J. M.; Jesser, W. A.; Murayama, M.

2004-05-01

Fractional forces and Brownian motion are expected to govern the behavior of nanoscale metallic solids in liquids, but such systems have not been studied. We investigated the motion of a crystalline Al nanosphere inside a partially molten Al-Si alloy particle, using an electron beam to both stimulate and observe the motion of the nanosphere. The irregular motion observed was quantified as antipersistant fractional Brownian motion. Analysis of possible phenomena contributing to the motion demonstrates that the incident electrons provide the fractional force that moves the Al nanosphere and that gravity and the oxide shell on the partially molten particle cause the antipersistant behavior.

On-line hyphenation of centrifugal partition chromatography and high pressure liquid chromatography for the fractionation of flavonoids from Hippophaë rhamnoides L. berries.

PubMed

Michel, Thomas; Destandau, Emilie; Elfakir, Claire

2011-09-09

Centrifugal Partition Chromatography (CPC), a liquid-liquid preparative chromatography using two immiscible solvent systems, benefits from numerous advantages for the separation or purification of synthetic or natural products. This study presents the on-line hyphenation of CPC-Evaporative Light Scattering Detector (CPC-ELSD) with High Performance Liquid Chromatography-UV (HPLC-UV) for the fractionation of flavonols from a solvent-free microwave extract of sea buckthorn (Hippophaë rhamnoides L., Elaeagnaceae) berries. An Arizona G system was used for the fractionation of flavonoids by CPC and a fused core Halo C18 column allowed the on-line analyses of collected fractions by HPLC. The on-line CPC/HPLC procedure allowed the simultaneous fractionation step at preparative scale combined with the HPLC analyses which provide direct fingerprint of collected fractions. Thus the crude extract was simplified and immediate information on the composition of fractions could be obtained. Furthermore, this methodology reduced the time of post-fractionation steps and facilitated identification of main molecules by Mass Spectrometry (MS). Rutin, isorhamnetin-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin-3-O-glucoside, isorhamnetin-rhamnoside, quercetin and isorhamnetin were identified. CPC-ELSD/HPLC-UV could be considered as a high-throughput technique for the guided fractionation of bioactive natural products from complex crude extracts. Copyright © 2011 Elsevier B.V. All rights reserved.

Preparation and evaluation of silica-UIO-66 composite as liquid chromatographic stationary phase for fast and efficient separation.

PubMed

Yan, Zhiming; Zheng, Jiangnan; Chen, Jinfeng; Tong, Ping; Lu, Minghua; Lin, Zian; Zhang, Lan

2014-10-31

A silica-UIO-66 composite was fabricated by a simple hydrothermal method and then applied as liquid chromatographic stationary phase for fast and efficient separation. X-ray diffraction patterns showed the presence of UIO-66 crystals in the silica-UIO-66 composites; while scanning electron microscope (SEM) images revealed that silica-UIO-66 composites were a homogeneous mixture of silica bead and UIO-66 crystals. A variety of substituted aromatics, chlorobenzene compounds and polycyclic aromatic hydrocarbons (PAHs) were used to evaluate the retention properties of the silica-UIO-66 composite packed column. Under the optimized conditions, baseline separation of ethylbenzene (EB) and styrene was obtained with high resolution and short retention time. In addition, the silica-UIO-66 composite packed column also showed some advantages in separation of positional isomers, with which baseline separation of EB and xylene, chlorotoluene and dichlorobenzene isomers was achieved. Moreover, the retention mechanisms of these compounds were also discussed in detail. The relative standard deviations (RSDs) for the separation of EB and xylene, chlorotoluene and dichlorobenzene isomers, as well as EB and styrene were 0.42-0.9%, 1.0-1.9%, 0.75-2.0%, and 0.9-2.1% for the retention time, peak area, peak height, and half peak width, respectively. The column efficiencies for EB, p-chlorotoluene, p-dichlorobenzene and styrene were 8780, 9060, 9990 and 5130 plates/m. The successful applications suggested high potentials of silica-MOFs composite as stationary phase for fast and efficient liquid chromatography separation. Copyright © 2014 Elsevier B.V. All rights reserved.

Secretory immunoglobulin purification from whey by chromatographic techniques.

PubMed

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

2017-08-15

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

Huygens Gas Chromatograph Mass Spectrometer Results from Titan

NASA Technical Reports Server (NTRS)

Niemann, Hasso

2008-01-01

The Huygens Probe executed a successful entry, descent and impact on the Saturnian moon of Titan on January 14, 2005. Gas Chromatograph Mass Spectrometer (GCMS) instrument conducted isotopic and compositional measurements throughout the two and one half hour descent from 146 km altitude, and on the surface for 69 minutes until loss of signal from the orbiting Cassini spacecraft. The GCMS incorporated a quadrupole mass filter with a secondary electron multiplier detection system. The gas sampling system provided continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the surface after impact. Data products from the GCMS included altitude profiles of the major atmospheric constituents dinitrogen (N2) and methane (CH4), isotope ratios of N-14/N-15, C-12/C-13, and D/H, mole fractions of radiogenic argon (Ar-40)and primordial argon Ar-36), and upper limits on the mole fractions of neon, krypton and xenon, which were found to be below the detection limit of the instrument or absent. Surface measurements confirmed the presence of ethane (C2H6) and cyanogen (C2N2). Later data products include the instrument response to surface outgassing of C2N2, C2H6, acetylene (C2H2),and carbon dioxide (CO2). More recent results include the detection of benzene (C6H6) and height profiles of molecular hydrogen (H2). Numerous other trace species evaporating from the surface were also identified using the GCMS data.

Determination and validation of a simple high-performance liquid chromatographic method for simultaneous assay of iprodione and vinclozolin in human urine.

PubMed

Carlucci, Giuseppe; Pasquale, Dorina Di; Ruggieri, Fabrizio; Mazzeo, Pietro

2005-12-15

A method based on solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) was developed for the simultaneous determination of 3-(3,5-diclorophenyl)-5-ethenyl-5-methyl-2,4-oxazolidinedione (vinclozolin) and 3-(3,5-diclorophenyl)-N-(1-methylethyl)-2,4-dioxo-1-imidazolidinecarboxamide (iprodione) in human urine. Urine samples containing vinclozolin and iprodione were collected by solid phase extraction using C(18) cartridges. The chromatographic separation was achieved on a Spherisorb ODS2 (250 mm x 4.6 mm, 5 microm) column with an isocratic mobile phase of acetonitrile-water (60:40, v/v). Detection was UV absorbance at 220 nm. The calibration graphs were linear from 30 to 1000 ng/mL for the two fungicides. Intra- and inter-day R.S.D. did not exceed 2.9%. The quantitation limit was 50 ng/mL for vinclozolin and 30 ng/mL for iprodione, respectively.

High-pressure liquid chromatography: A brief introduction and its application in analyzing the degradation of a C-ether (Thio-ether) liquid lubricant

NASA Technical Reports Server (NTRS)

1983-01-01

The general principles of classical liquid chromatography and high pressure liquid chromatography (HPLC) are reviewed, and their advantages and disadvantages are compared. Several chromatographic techniques are reviewed, and the analytical separation of a C-ether liquid lubricant by each technique is illustrated. A practical application of HPLC is then demonstrated by analyzing a degraded C-ether liquid lubricant from full scale, high temperature bearing tests.

Modeling Aquatic Toxicity through Chromatographic Systems.

PubMed

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

2017-08-01

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

Pig slurry acidification and separation techniques affect soil N and C turnover and N2O emissions from solid, liquid and biochar fractions.

PubMed

Gómez-Muñoz, B; Case, S D C; Jensen, L S

2016-03-01

The combined effects of pig slurry acidification, subsequent separation techniques and biochar production from the solid fraction on N mineralisation and N2O and CO2 emissions in soil were investigated in an incubation experiment. Acidification of pig slurry increased N availability from the separated solid fractions in soil, but did not affect N2O and CO2 emissions. However acidification reduced soil N and C turnover from the liquid fraction. The use of more advanced separation techniques (flocculation and drainage > decanting centrifuge > screw press) increased N mineralisation from acidified solid fractions, but also increased N2O and CO2 emissions in soil amended with the liquid fraction. Finally, the biochar production from the solid fraction of pig slurry resulted in a very recalcitrant material, which reduced N and C mineralisation in soil compared to the raw solid fractions. Copyright © 2015 Elsevier Ltd. All rights reserved.

Measurement uncertainty of liquid chromatographic analyses visualized by Ishikawa diagrams.

PubMed

Meyer, Veronika R

2003-09-01

Ishikawa, or cause-and-effect diagrams, help to visualize the parameters that influence a chromatographic analysis. Therefore, they facilitate the set up of the uncertainty budget of the analysis, which can then be expressed in mathematical form. If the uncertainty is calculated as the Gaussian sum of all uncertainty parameters, it is necessary to quantitate them all, a task that is usually not practical. The other possible approach is to use the intermediate precision as a base for the uncertainty calculation. In this case, it is at least necessary to consider the uncertainty of the purity of the reference material in addition to the precision data. The Ishikawa diagram is then very simple, and so is the uncertainty calculation. This advantage is given by the loss of information about the parameters that influence the measurement uncertainty.

Determination of aromatics and olefins in wide-boiling petroleum fractions

NASA Technical Reports Server (NTRS)

Spakowski, A E; Evans, A; Hibbard, R R

1950-01-01

A chromatographic method is described herein for the analysis of aromatics and olefins in wide boiling petroleum fractions. The fuel is split into four fractions: nonaromatic, intermediate, pure aromatic, and wash. The analysis, which need be run only on the intermediate cut to determine aromatics in the fuel, is based on specific dispersion. With analysis times of less than 8 hours, accuracies of 1 percent were attained.

Estimations of temperature deviations in chromatographic columns using isenthalpic plots. I. Theory for isocratic systems.

PubMed

Tarafder, Abhijit; Iraneta, Pamela; Guiochon, Georges; Kaczmarski, Krzysztof; Poe, Donald P

2014-10-31

We propose to use constant enthalpy or isenthalpic diagrams as a tool to estimate the extent of the temperature variations caused by the mobile phase pressure drop along a chromatographic column, e.g. of its cooling in supercritical fluid and its heating in ultra-performance liquid chromatography. Temperature strongly affects chromatographic phenomena. Any of its variations inside the column, whether intended or not, can lead to significant changes in separation performance. Although instruments use column ovens in order to keep constant the column temperature, operating conditions leading to a high pressure drop may cause significant variations of the column temperature, both in the axial and the radial directions, from the set value. Different ways of measuring these temperature variations are available but they are too inconvenient to be employed in many practical situations. In contrast, the thermodynamic plot-based method that we describe here can easily be used with only a ruler and a pencil. They should be helpful in developing methods or in analyzing results in analytical laboratories. Although the most effective application area for this approach should be SFC (supercritical fluid chromatography), it can be applied to any chromatographic conditions in which temperature variations take place along the column due to the pressure drop, e.g. in ultra-high pressure liquid chromatography (UHPLC). The method proposed here is applicable to isocractic conditions only. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid and improved gas-liquid chromatography technique for detection of hippurate hydrolysis by Campylobacter jejuni and Campylobacter coli.

PubMed Central

Bär, W; Fricke, G

1987-01-01

A gas-liquid chromatographic method which requires no chloroform extraction of the split products has been investigated for the detection of hippurate hydrolysis by Campylobacter spp. This technique gave better reproducibility than other tests also used in this study and allows the routine use of the gas-liquid chromatographic method for identification of Campylobacter isolates. PMID:3654950

Simple high-performance liquid chromatographic method to monitor vigabatrin, and preliminary review of concentrations determined in epileptic patients.

PubMed

George, S; Gill, L; Braithwaite, R A

2000-05-01

A simple and rapid high-performance liquid chromatographic method has been developed for the determination of vigabatrin concentrations in plasma or serum. The assay uses only 100 microL of specimen and has been found to be linear over a concentration range of 1 to 50 mg/L. The limit of detection has been determined as 1 mg/L, and the between-batch coefficient of variation for the two internal quality controls routinely analysed (n = 33) has been found to be less than 5%. There was no evidence of interferences in the assay from other commonly prescribed anti-epileptic drugs. This method has been applied to routine clinical specimens to determine the concentration of vigabatrin in 47 patient specimens over a 12-month period. It was found that only 63% of the male group and 53% of the female group were within the proposed target concentration of 5 to 35 mg/L. In addition, it was found that 26% of the male group and 36% of the female group were found to have concentrations below 5 mg/L, which may indicate lack of compliance and/or lack of therapeutic efficacy of treatment.

Post-synthetic modification of MIL-101(Cr) with pyridine for high-performance liquid chromatographic separation of tocopherols.

PubMed

Yang, Fang; Yang, Cheng-Xiong; Yan, Xiu-Ping

2015-05-01

Effective separation of tocopherols is challenging and significant due to their structural similarity and important biological role. Here we report the post-synthetic modification of metal-organic framework (MOF) MIL-101(Cr) with pyridine for high-performance liquid chromatographic (HPLC) separation of tocopherols. Baseline separation of four tocopherols was achieved on a pyridine-grafted MIL-101(Cr) packed column within 10 min using hexane/isopropanol (96:4, v/v) as the mobile phase at a flow rate of 0.5 mL min(-1). The pyridine-grafted MIL-101(Cr) packed column gave high column efficiency (85,000 plates m(-1) for δ-tocopherol) and good precision (0.2-0.3% for retention time, 1.8-3.4% for peak area, 2.6-2.7% for peak height), and also offered much better performance than unmodified MIL-101(Cr) and commercial amino-bonded silica packed column for HPLC separation of tocopherols. The results not only show the promising application of pyridine-grafted MIL-101(Cr) as a novel stationary phase for HPLC separation of tocopherols, but also reveal a facile post-modification of MOFs to expand the application of MOFs in separation sciences. Copyright © 2015 Elsevier B.V. All rights reserved.

Chromatographic separation of fructose from date syrup.

PubMed

Al Eid, Salah M

2006-01-01

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

High-performance liquid chromatographic method for the simultaneous determination of nalbuphine and its prodrug, sebacoyl dinalbuphine ester, in dog plasma and application to pharmacokinetic studies in dogs.

PubMed

Pao, L H; Hsiong, C H; Hu, O Y; Ho, S T

2000-09-15

For the determination of nalbuphine and its long acting prodrug, sebacoyl dinalbuphine ester (SDN), in biological samples, a reversed-phase high-performance liquid chromatographic method using dual detectors was established. Ultraviolet and fluorescence detectors were connected in series for determining SDN and nalbuphine, respectively. The two analytes and internal standard were extracted from plasma by alkaline liquid-liquid extraction using n-hexane-isoamyl alcohol (9:1, v/v). The calibration curve for nalbuphine was linear over the range from 10 to 2,500 ng/ml, while the range was 25 to 2,500 ng/ml for SDN. The within- and between-day precision and accuracy were all within 10% for both nalbuphine and SDN over these concentrations. The method was applied successfully to a pharmacokinetic study of SDN administered at 20 mg/kg to two beagle dogs. Pharmacokinetic analysis revealed that SDN followed a linear one-compartment model with an elimination half-life of 74.7 min. Formation of nalbuphine after intravenous administration of SDN was observed in the first time point sample (5 min). These results indicate that SDN is rapidly metabolized to its active moiety, nalbuphine, in dogs and no other metabolites are detected in plasma.

Variation in trace element content of magnetite crystallized from a fractionating sulfide liquid, Sudbury, Canada: Implications for provenance discrimination

NASA Astrophysics Data System (ADS)

Dare, Sarah A. S.; Barnes, Sarah-Jane; Beaudoin, Georges

2012-07-01

Laser ablation ICP-MS analysis has been applied to many accessory minerals in order to understand better the process by which the rock formed and for provenance discrimination. We have determined trace element concentrations of Fe-oxides in massive sulfides that form Ni-Cu-PGE deposits at the base of the Sudbury Igneous Complex in Canada. The samples represent the crystallization products of fractionating sulfide liquids and consist of early-forming Fe-rich monosulfide solution (MSS) cumulates and residual Cu-rich intermediate solid solution (ISS). This study shows that Fe-oxide geochemistry is a sensitive petrogenetic indicator for the degree of fractionation of the sulfide liquid and provides an insight into the partitioning of elements between sulfide and Fe-oxide phases. In addition, it is useful in determining the provenance of detrital Fe-oxide. In a sulfide melt, all lithophile elements (Cr, Ti, V, Al, Mn, Sc, Nb, Ga, Ge, Ta, Hf, W and Zr) are compatible into Fe-oxide. The concentrations of these elements are highest in the early-forming Fe-oxide (titanomagnetite) which crystallized with Fe-rich MSS. Upon the continual crystallization of Fe-oxide from the sulfide liquid, the lithophile elements gradually decrease so that late-forming Fe-oxide (magnetite), which crystallized from the residual Cu-rich liquid, is depleted in these elements. This behavior is in contrast with Fe-oxides that crystallized from a fractionating silicate melt, whereby the concentration of incompatible elements, such as Ti, increases rather than decreases. The behavior of the chalcophile elements in magnetite is largely controlled by the crystallization of the sulfide minerals with only Ni, Co, Zn, Mo, Sn and Pb present above detection limit in magnetite. Nickel, Mo and Co are compatible in Fe-rich MSS and thus the co-crystallizing Fe-oxide is depleted in these elements. In contrast, magnetite that crystallized later from the fractionated liquid with Cu-rich ISS is enriched in Ni, Mo

Microfabricated packed gas chromatographic column

DOEpatents

Kottenstette, Richard; Matzke, Carolyn M.; Frye-Mason, Gregory C.

2003-12-16

A new class of miniaturized gas chromatographic columns has been invented. These chromatographic columns are formed using conventional micromachining techniques, and allow packed columns having lengths on the order of a meter to be fabricated with a footprint on the order of a square centimeter.

Optimization and validation of a high-performance liquid chromatographic method with UV detection for the determination of ketoconazole in canine plasma.

PubMed

Vertzoni, M V; Reppas, C; Archontaki, H A

2006-07-24

An isocratic high-performance liquid chromatographic method with detection at 240 nm was developed, optimized and validated for the determination of ketoconazole in canine plasma. 9-Acetylanthracene was used as internal standard. A Hypersil BDS RP-C18 column (250 mm x 4.6 mm, 5 microm particle size), was equilibrated with a mobile phase composed of methanol, water and diethylamine 74:26:0.1 (v/v/v). Its flow rate was 1 ml/min. The elution time for ketoconazole and 9-acetylanthracene was approximately 9 and 8 min, respectively. Calibration curves of ketoconazole in plasma were linear in the concentration range of 0.015-10 microg/ml. Limits of detection and quantification in plasma were 5 and 15 ng/ml, respectively. Recovery was greater than 95%. Intra- and inter-day relative standard deviation for ketoconazole in plasma was less than 3.1 and 4.7%, respectively. This method was applied to the determination of ketoconazole plasma levels after administration of a commercially available tablet to dogs.

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

PubMed

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

2017-04-01

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

Chromatographic and electrophoretic approaches in ink analysis.

PubMed

Zlotnick, J A; Smith, F P

1999-10-15

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

Differentiation of Panax quinquefolius grown in United States and China using LC/MS-based chromatographic fingerprinting and metabolomic approaches

USDA-ARS?s Scientific Manuscript database

American ginseng (Panax quinquefolius) is one of the most commonly used herbal medicines in the world. Discriminating between P. quinquefolius grown in different countries is difficult using the traditional quantitation methods. In this study, a liquid chromatographic mass spectrometry (LC-MS) fing...

Identification of Intact High Molecular Weight Glutenin Subunits from the Wheat Proteome Using Combined Liquid Chromatography-Electrospray Ionization Mass Spectrometry

PubMed Central

Lagrain, Bert; Brunnbauer, Markus; Rombouts, Ine; Koehler, Peter

2013-01-01

The present paper describes a method for the identification of intact high molecular weight glutenin subunits (HMW-GS), the quality determining proteins from the wheat storage proteome. The method includes isolation of HMW-GS from wheat flour, further separation of HMW-GS by reversed-phase high-performance liquid chromatography (RP-HPLC), and their subsequent molecular identification with electrospray ionization mass spectrometry using a quadrupole-time-of-flight mass analyzer. For HMW-GS isolation, wheat proteins were reduced and extracted from flour with 50% 1-propanol containing 1% dithiothreitol. HMW-GS were then selectively precipitated from the protein mixture by adjusting the 1-propanol concentration to 60%. The composition of the precipitated proteins was first evaluated by sodium dodecyl sulfate-polyacrylamide gel electrophoresis with Coomassie staining and RP-HPLC with ultraviolet detection. Besides HMW-GS (≥65%), the isolated proteins mainly contained ω5-gliadins. Secondly, the isolated protein fraction was analyzed by liquid chromatography-mass spectrometry. Optimal chromatographic separation of HMW-GS from the other proteins in the isolated fraction was obtained when the mobile phase contained 0.1% trifluoroacetic acid as ion-pairing agent. Individual HMW-GS were then identified by determining their molecular masses from the high-resolution mass spectra and comparing these with theoretical masses calculated from amino acid sequences. Using formic acid instead of trifluoroacetic acid in the mobile phase increased protein peak intensities in the base peak mass chromatogram. This allowed the detection of even traces of other wheat proteins than HMW-GS in the isolated fraction, but the chromatographic separation was inferior with a major overlap between the elution ranges of HMW-GS and ω-gliadins. Overall, the described method allows a rapid assessment of wheat quality through the direct determination of the HMW-GS composition and offers a basis for

Analysis of Poly-β-Hydroxybutyrate in Rhizobium japonicum Bacteroids by Ion-Exclusion High-Pressure Liquid Chromatography and UV Detection †

PubMed Central

Karr, Dale B.; Waters, James K.; Emerich, David W.

1983-01-01

Ion-exclusion high-pressure liquid chromatography (HPLC) was used to measure poly-β-hydroxybutyrate (PHB) in Rhizobium japonicum bacteroids. The products in the acid digest of PHB-containing material were fractionated by HPLC on Aminex HPX-87H ion-exclusion resin for organic acid analysis. Crotonic acid formed from PHB during acid digestion was detected by its intense absorbance at 210 nm. The Aminex-HPLC method provides a rapid and simple chromatographic technique for routine analysis of organic acids. Results of PHB analysis by Aminex-HPLC were confirmed by gas chromatography and spectrophotometric analysis. PMID:16346443

Quantitative analysis of matrine in liquid crystalline nanoparticles by HPLC.

PubMed

Peng, Xinsheng; Li, Baohong; Hu, Min; Ling, Yahao; Tian, Yuan; Zhou, Yanxing; Zhou, Yanfang

2014-01-01

A reversed-phase high-performance liquid chromatographic method has been developed to quantitatively determine matrine in liquid crystal nanoparticles. The chromatographic method is carried out using an isocratic system. The mobile phase was composed of methanol-PBS(pH6.8)-triethylamine (50 : 50 : 0.1%) with a flow rate of 1 mL/min with SPD-20A UV/vis detector and the detection wavelength was at 220 nm. The linearity of matrine is in the range of 1.6 to 200.0  μ g/mL. The regression equation is y = 10706x - 2959 (R (2) = 1.0). The average recovery is 101.7%; RSD = 2.22%  (n = 9). This method provides a simple and accurate strategy to determine matrine in liquid crystalline nanoparticle.

High-temperature two-dimensional liquid chromatography of ethylene-vinylacetate copolymers.

PubMed

Ginzburg, Anton; Macko, Tibor; Dolle, Volker; Brüll, Robert

2010-10-29

Temperature rising elution fractionation hyphenated to size exclusion chromatography (TREF×SEC) is a routine technique to determine the chemical heterogeneity of semicrystalline olefin copolymers. Its applicability is limited to well crystallizing samples. High-temperature two-dimensional liquid chromatography, HT 2D-LC, where the chromatographic separation by HPLC is hyphenated to SEC (HPLC×SEC) holds the promise to separate such materials irrespective of their crystallizability. A model blend consisting of ethylene-vinyl acetate (EVA) copolymers covering a broad range of chemical composition distribution including amorphous and semicrystalline copolymers and a polyethylene standard was separated by HT 2D-LC at 140°C. Both axes of the contour plot, i.e. the compositional axis from the HPLC and the molar mass axis from the SEC separation were calibrated for the first time. Therefore, a new approach to determine the void and dwell volume of the developed HT 2D-LC instrument was applied. The results from the HT 2D-LC separation are compared to those from a cross-fractionation (TREF×SEC) experiment. Copyright © 2010. Published by Elsevier B.V.

Effects of solid/liquid phase fractionation on pH and aqueous species molality in subduction zone fluids

NASA Astrophysics Data System (ADS)

Zhong, X.; Galvez, M. E.

2017-12-01

Metamorphic fluids are a crucial ingredient of geodynamic evolution, i.e. heat transfer, rock mechanics and metamorphic/metasomatic reactions. During crustal evolution at elevated P and T, rock forming components can be effectively fractionated from the reactive rock system by at least two processes: 1. extraction from porous rocks by liquid phases such as solute-bearing (e.g. Na+, Mg2+) aqueous fluids or partial melts. 2. isolation from effective bulk rock composition due to slow intragranular diffusion in high-P refractory phases such as garnet. The effect of phase fractionation (garnet, partial melt and aqueous species) on fluid - rock composition and properties remain unclear, mainly due to a high demand in quantitative computations of the thermodynamic interactions between rocks and fluids over a wide P-T range. To investigate this problem, we build our work on an approach initially introduced by Galvez et al., (2015) with new functionalities added in a MATLAB code (Rubisco). The fluxes of fractionated components in fluid, melt and garnet are monitored along a typical prograde P-T path for a model crustal pelite. Some preliminary results suggest a marginal effect of fractionated aqueous species on fluid and rock properties (e.g. pH, composition), but the corresponding fluxes are significant in the context of mantle wedge metasomatism. Our work provides insight into the role of high-P phase fractionation on mass redistribution between the surface and deep Earth in subduction zones. Existing limitations relevant to our liquid/mineral speciation/fractionation model will be discussed as well. ReferencesGalvez, M.E., Manning, C.E., Connolly, J.A.D., Rumble, D., 2015. The solubility of rocks in metamorphic fluids: A model for rock-dominated conditions to upper mantle pressure and temperature. Earth Planet. Sci. Lett. 430, 486-498.

Chromatographic and mass spectral methods of identification for the side-chain and ring regioisomers of methylenedioxymethamphetamine.

PubMed

Aalberg, L; DeRuiter, J; Noggle, F T; Sippola, E; Clark, C R

2000-08-01

The popular drug of abuse 3,4-methylenedioxymethamphetamine (MDMA) is one of a total of 10 regioisomeric 2,3- and 3,4-methylenedioxyphenethylamines of MW 193 that yields regioisomeric fragment ions with equivalent mass (m/z 58 and 135/136) in the electron-impact (EI) mass spectrum. Thus, these 10 methylenedioxyphenethylamines are uniquely isomeric; they have the same molecular weight and equivalent major fragments in their mass spectra. The specific identification of one of these compounds (i.e., Ecstasy or 3,4-MDMA) in a forensic drug sample depends upon the analyst's ability to eliminate the other regioisomers as possible interfering or coeluting substances. This study reports the synthesis, chemical properties, spectral characterization, and chromatographic analysis of these 10 unique regioisomers. The ten 2,3- and 3,4-regioisomers of MDMA are synthesized from commercially available precursor chemicals. In the EI mass spectra, the side-chain regioisomers show some variation in the relative intensity of the major ions, with the exception of only one or two minor ions that might be considered side-chain specific fragments. The position of substitution for the methylenedioxy ring is not easily determined by mass spectral techniques, and the ultimate identification of any one of these amines with the elimination of the other nine must depend heavily upon chromatographic methods. The chromatographic separation of these 10 uniquely regioisomeric amines are studied using reversed-phase liquid chromatographic methods with gradient elution and gas chromatographic techniques with temperature program optimization.

Development and validation of liquid chromatographic and UV derivative spectrophotometric methods for the determination of famciclovir in pharmaceutical dosage forms.

PubMed

Srinubabu, Gedela; Sudharani, Batchu; Sridhar, Lade; Rao, Jvln Seshagiri

2006-06-01

A high-performance liquid chromatographic method and a UV derivative spectrophotometric method for the determination of famciclovir, a highly active antiviral agent, in tablets were developed in the present work. The various parameters, such as linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. HPLC was carried out by using the reversed-phase technique on an RP-18 column with a mobile phase composed of 50 mM monobasic phosphate buffer and methanol (50 : 50; v/v), adjusted to pH 3.05 with orthophosphoric acid. The mobile phase was pumped at a flow rate of 1 ml/min and detection was made at 242 nm with UV dual absorbance detector. The first derivative UV spectrophotometric method was performed at 226.5 nm. Statistical analysis was done by Student's t-test and F-test, which showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and therefore can be used for its Intended purpose.

Precolumn derivatization followed by liquid chromatographic separation and determination of tramiprosate in rat plasma by fluorescence detector: application to pharmacokinetics.

PubMed

Rao, R Nageswara; Maurya, Pawan K; Shinde, Dhananjay D; Khalid, Sara

2011-05-15

Alzheimer disease (AD) is characterized pathologically by extracellular amyloid deposits composed of amyloid β (Aβ) protein. A simple and rapid method using HPLC with fluorescence detector was developed and validated for determination of tramiprosate in rat plasma. Pre-column derivatization of the deproteinized rat plasma was carried out using o-phthaldialdehyde (OPA) as a fluorescent reagent in presence of 3-mercaptopropionic acid. The liquid chromatographic separation was achieved on a Kromasil C18 column using methanol:acetonitrile: 20 mM phosphate buffer pH 7.5 (8.0:17.5:74.5 v/v/v) as a mobile phase in an isocratic elution mode. The eluents were monitored by a fluorescence detector set at 330 and 450 nm of excitation and emission wavelength respectively. Vigabatrin was used as an internal standard. The method was linear within the range 30.0-1000.0 ng/mL. Design of experiments (DOE) was used to evaluate the robustness of the method. The developed method was applied to study the pharmacokinetics of tramiprosate in rats. Copyright © 2011. Published by Elsevier B.V.

Chaotropic salts in liquid chromatographic method development for the determination of pramipexole and its impurities following quality-by-design principles.

PubMed

Vemić, Ana; Rakić, Tijana; Malenović, Anđelija; Medenica, Mirjana

2015-01-01

The aim of this paper is to present a development of liquid chromatographic method when chaotropic salts are used as mobile phase additives following the QbD principles. The effect of critical process parameters (column chemistry, salt nature and concentration, acetonitrile content and column temperature) on the critical quality attributes (retention of the first and last eluting peak and separation of the critical peak pairs) was studied applying the design of experiments-design space methodology (DoE-DS). D-optimal design is chosen in order to simultaneously examine both categorical and numerical factors in minimal number of experiments. Two ways for the achievement of quality assurance were performed and compared. Namely, the uncertainty originating from the models was assessed by Monte Carlo simulations propagating the error equal to the variance of the model residuals and propagating the error originating from the model coefficients' calculation. The baseline separation of pramipexole and its five impurities is achieved fulfilling all the required criteria while the method validation proved its reliability. Copyright © 2014 Elsevier B.V. All rights reserved.

A Gas-Liquid Chromatographic Examination of Stilbene Derivatives

Treesearch

Richard W. Hemingway; W. E. Hillis; K Burerton

1970-01-01

Trimethylsilyl ether derivatives of twenty hydroxystilbenes were separated by gas-liquid chromatography on Apiezon-L, OV-1, OV-17, and SE-54. Relative retention times were highly dependent upon the degree of hydroxylation and methoxylation, the positions of these groups and on cis-trans...

Principles of qualitative analysis in the chromatographic context.

PubMed

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

2007-07-27

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

High-throughput, Highly Sensitive Analyses of Bacterial Morphogenesis Using Ultra Performance Liquid Chromatography*

PubMed Central

Desmarais, Samantha M.; Tropini, Carolina; Miguel, Amanda; Cava, Felipe; Monds, Russell D.; de Pedro, Miguel A.; Huang, Kerwyn Casey

2015-01-01

The bacterial cell wall is a network of glycan strands cross-linked by short peptides (peptidoglycan); it is responsible for the mechanical integrity of the cell and shape determination. Liquid chromatography can be used to measure the abundance of the muropeptide subunits composing the cell wall. Characteristics such as the degree of cross-linking and average glycan strand length are known to vary across species. However, a systematic comparison among strains of a given species has yet to be undertaken, making it difficult to assess the origins of variability in peptidoglycan composition. We present a protocol for muropeptide analysis using ultra performance liquid chromatography (UPLC) and demonstrate that UPLC achieves resolution comparable with that of HPLC while requiring orders of magnitude less injection volume and a fraction of the elution time. We also developed a software platform to automate the identification and quantification of chromatographic peaks, which we demonstrate has improved accuracy relative to other software. This combined experimental and computational methodology revealed that peptidoglycan composition was approximately maintained across strains from three Gram-negative species despite taxonomical and morphological differences. Peptidoglycan composition and density were maintained after we systematically altered cell size in Escherichia coli using the antibiotic A22, indicating that cell shape is largely decoupled from the biochemistry of peptidoglycan synthesis. High-throughput, sensitive UPLC combined with our automated software for chromatographic analysis will accelerate the discovery of peptidoglycan composition and the molecular mechanisms of cell wall structure determination. PMID:26468288

Multiple-channel ultra-violet absorbance detector for two-dimensional chromatographic separations.

PubMed

Lynch, Kyle B; Yang, Yu; Ren, Jiangtao; Liu, Shaorong

2018-05-01

In recent years, much research has gone into developing online comprehensive two-dimensional liquid chromatographic systems allowing for high peak capacities in comparable separation times to that of one-dimensional liquid chromatographic systems. However, the speed requirements in the second dimension (2nd-D) still remain one challenge for complex biological samples due to the current configuration of two column/two detector systems. Utilization of multiple 2nd-D columns can mitigate this challenge. To adapt this approach, we need a multiple channel detector. Here we develop a versatile multichannel ultraviolet (UV) light absorbance detector that is capable of simultaneously monitoring separations in 12 columns. The detector consists of a deuterium lighthouse, a flow cell assembly (a 13-channel flow cell fitted with a 13-photodiode-detection system), and a data acquisition and monitoring terminal. Through the use of a custom high optical quality furcated fiber to improve light transmission, precise machining of a flow cell to reduce background stray light through precision alignment, and sensitive electronic circuitry to reduce electronic noise through an active low pass filter, the background noise level is measured in the tens of µAU. We obtain a linear dynamic range of close to three orders of magnitude. Compared to a commercialized multichannel UV light absorbance detector like the Waters 2488 UV/Vis, our device provides an increase in channel detection while residing within the same noise region and linear range. Copyright © 2018 Elsevier B.V. All rights reserved.

An integrated process for the recovery of high added-value compounds from olive oil using solid support free liquid-liquid extraction and chromatography techniques.

PubMed

Angelis, Apostolis; Hamzaoui, Mahmoud; Aligiannis, Nektarios; Nikou, Theodora; Michailidis, Dimitris; Gerolimatos, Panagiotis; Termentzi, Aikaterini; Hubert, Jane; Halabalaki, Maria; Renault, Jean-Hugues; Skaltsounis, Alexios-Léandros

2017-03-31

An integrated extraction and purification process for the direct recovery of high added value compounds from extra virgin olive oil (EVOO) is proposed by using solid support free liquid-liquid extraction and chromatography techniques. Two different extraction methods were developed on a laboratory-scale Centrifugal Partition Extractor (CPE): a sequential strategy consisting of several "extraction-recovery" cycles and a continuous strategy based on stationary phase co-current elution. In both cases, EVOO was used as mobile phase diluted in food grade n-hexane (feed mobile phase) and the required biphasic system was obtained by adding ethanol and water as polar solvents. For the sequential process, 17.5L of feed EVOO containing organic phase (i.e. 7L of EVOO treated) were extracted yielding 9.5g of total phenolic fraction corresponding to a productivity of 5.8g/h/L of CPE column. Regarding the second approach, the co-current process, 2L of the feed oil phase (containing to 0.8L of EVOO) were treated at 100mL/min yielding 1.03g of total phenolic fraction corresponding to a productivity of 8.9g/h/L of CPE column. The total phenolic fraction was then fractionated by using stepwise gradient elution Centrifugal Partition Chromatography (CPC). The biphasic solvent systems were composed of n-hexane, ethyl acetate, ethanol and water in different proportions (X/Y/2/3, v/v). In a single run of 4h on a column with a capacity of 1L, 910mg of oleocanthal, 882mg of oleacein, 104mg of hydroxytyrosol were successfully recovered from 5g of phenolic extract with purities of 85%, 92% and 90%, respectively. CPC fractions were then submitted to orthogonal chromatographic steps (adsorption on silica gel or size exclusion chromatography) leading to the isolation of additional eleven compounds belonging to triterpens, phenolic compounds and secoiridoids. Among them, elenolic acid ethylester was found to be new compound. Thin Layer Chromatography (TLC), Nuclear magnetic Resonance (NMR) and

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

USGS Publications Warehouse

Hedley, Arthur G.; Fishman, Marvin J.

1982-01-01

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

Liquid chromatographic determination of para-toluenesulfonamide in edible fillet tissues from three species of fish

USGS Publications Warehouse

Meinertz, J.R.; Schmidt, L.J.; Stehly, G.R.; Gingerich, W.H.

1999-01-01

Chloramine-T (N-sodium-N-chloro-p-toluene-sulfonamide) is a candidate therapeutic drug for treating bacterial gill disease, a predominant disease of a variety of fish species. Research has been initiated to obtain the U.S. Food and Drug Administration's (FDA) approval for the use of chloramine-T on a variety of fish species. An attribute of a therapeutic aquaculture drug that must be characterized before the FDA approves its use is depletion of the drug's marker residue (the drug's parent compound or metabolite of highest concentration in an edible tissue). Para-Toluenesulfonamide (p-TSA) is the primary degradation product and marker residue for chloramine-T in rainbow trout. To conduct residue depletion studies for chloramine-T in fish, a robust analytical method sensitive and specific for p-TSA residues in edible fillet tissue from a variety of fish was required. Homogenized fillet tissues from rainbow trout (Oncorhynchus mykiss), walleye (Stizostedion vitreum), and channel catfish (Ictalurus punctatus) were fortified at nominal p-TSA concentrations of 17, 67, 200, 333, and 1000 ng/g. Samples were analyzed by isocratic reversed-phase liquid chromatography (LC) with absorbance detection at 226 nm. Mean recoveries of p-TSA ranged from 77 to 93.17%; relative standard deviations ranged from 1.5 to 14%; method quantitation limits ranged from 13 to 18 ng/g; and method detection limits ranged from 3.8 to 5.2 ng/g. The LC parameters produced p-TSA peaks without coelution of endogenous compounds and excluded chromatographic interference from at least 20 chemicals and drugs of potential use in aquaculture.

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

PubMed

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

2010-12-15

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

UPLC and LC-MS studies on degradation behavior of irinotecan hydrochloride and development of a validated stability-indicating ultra-performance liquid chromatographic method for determination of irinotecan hydrochloride and its impurities in pharmaceutical dosage forms.

PubMed

Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Sunil P

2012-10-01

The objective of the current investigation was to study the degradation behavior of irinotecan hydrochloride under different International Conference on Harmonization (ICH) recommended stress conditions using ultra-performance liquid chromatography and liquid chromatography-mass spectrometry and to establish a validated stability-indicating reverse-phase ultra-performance liquid chromatographic method for the quantitative determination of irinotecan hydrochloride and its seven impurities and degradation products in pharmaceutical dosage forms. Irinotecan hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Irinotecan hydrochloride was found to degrade significantly in oxidative and base hydrolysis and photolytic degradation conditions. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating power of the method. Chromatographic separation was achieved on a Waters Acquity BEH C8 (100 × 2.1 mm) 1.7-µm column with a mobile phase containing a gradient mixture of solvent A (0.02M KH(2)PO(4) buffer, pH 3.4) and solvent B (a mixture of acetonitrile and methanol in the ratio of 62:38 v/v). The mobile phase was delivered at a flow rate of 0.3 mL/min with ultraviolet detection at 220 nm. The run time was 8 min, within which irinotecan and its seven impurities and degradation products were satisfactorily separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of irinotecan hydrochloride in pharmaceutical dosage forms.

The Ackley City Batholith, southeastern Newfoundland: Evidence for crystal versus liquid-state fractionation

NASA Astrophysics Data System (ADS)

Whalen, J. B.

1983-08-01

The 345 ± 10 Ma old composite Ackley City Batholith of southeastern Newfoundland, consists largely of very felsic K-feldspar megacrystic granite and alaskite. Spatially related to the southeast contact of the alaskite are younger aplites and pegmatite, intrusive phases which are interpreted to be pan of a tilted, high level roof zone complex to the batholith. The compositions of the alaskite and roof zone complex define major and trace element gradients similar to those in voluminous high-silica eruptive suites; i.e., the alaskite is more chemically evolved (higher in Rb, lower in Ca, Fe, Mn, Ti, P, Sr, Ba and LREE) toward the roof. Apparently these chemical gradients in the batholith are restricted to the top 2 to 3 kms of the former magma chamber. Fractional crystallization is a plausible process for generating the chemical dispersion in the granites, although very high feldspar partition coefficients for Ba, Sr and Eu are required to generate the observed chemical gradients by a reasonable degree of fractional crystallization. Restriction of crystal fractionation to near the roof of the batholith may reflect a decreased viscosity which would facilitate crystal-liquid separation by processes such as filter pressing, flow differentiation or convective fractionation. The chemical gradients in these granites closely resemble those attributed in high-silica volcanics to the process of thermogravitational diffusion (TGD). Compositional gradients in the upper portion of a magma chamber are consistent with the TGD model. This model, although still poorly understood, is, like fractional crystallization, a plausible mechanism to generate the chemical features of the Ackley City granites.

Fractionalized Fermi liquid with bosonic chargons as a candidate for the pseudogap metal

NASA Astrophysics Data System (ADS)

Chatterjee, Shubhayu; Sachdev, Subir

2016-11-01

Doping a Mott-insulating Z2 spin liquid can lead to a fractionalized Fermi liquid (FL*). Such a phase has several favorable features that make it a candidate for the pseudogap metal for the underdoped cuprates. We focus on a particular, simple Z2-FL* state which can undergo a confinement transition to a spatially uniform superconductor which is smoothly connected to the "plain vanilla" BCS superconductor with d -wave pairing. Such a transition occurs by the condensation of bosonic particles carrying +e charge but no spin ("chargons"). We show that modifying the dispersion of the bosonic chargons can lead to confinement transitions with charge density waves and pair density waves at the same wave vector K , coexisting with d -wave superconductivity. We also compute the evolution of the Hall number in the normal state during the transition from the plain vanilla FL* state to a Fermi liquid, and argue, following Coleman, Marston, and Schofield [Phys. Rev. B 72, 245111 (2005), 10.1103/PhysRevB.72.245111], that it exhibits a discontinuous jump near optimal doping. We note the distinction between these results and those obtained from models of the pseudogap with fermionic chargons.

Bio-oil fractionation and condensation

DOEpatents

Brown, Robert C; Jones, Samuel T; Pollard, Anthony

2013-07-02

A method of fractionating bio-oil vapors which involves providing bio-oil vapors comprising bio-oil constituents is described. The bio-oil vapors are cooled in a first stage which comprises a condenser having passages for the bio-oil separated by a heat conducting wall from passages for a coolant. The coolant in the condenser of the first stage is maintained at a substantially constant temperature, set at a temperature in the range of 75 to 100.degree. C., to condense a first liquid fraction of liquefied bio-oil constituents in the condenser of the first stage. The first liquid fraction of liquified bio-oil constituents from the condenser in the first stage is collected. Also described are steps for subsequently recovering further liquid fractions of liquefied bio-oil constituents. Particular compositions of bio-oil condensation products are also described.

Isotope Fractionation by Diffusion in Liquids (Final Technical Report)

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

Richter, Frank

The overall objective of the DOE-funded research by grant DE-FG02-01ER15254 was document and quantify kinetic isotope fractionations during chemical and thermal (i.e., Soret) diffusion in liquids (silicate melts and water) and in the later years to include alloys and major minerals such as olivine and pyroxene. The research involved both laboratory experiments and applications to natural settings. The key idea is that major element zoning on natural geologic materials is common and can arise for either changes in melt composition during cooling and crystallization or from diffusion. The isotope effects associated with diffusion that we have documented are the keymore » for determining whether or not the zoning observed in a natural system was the result of diffusion. Only in those cases were the zoning is demonstrably due to diffusion can use independently measured rates of diffusion to constrain the thermal evolution of the system.« less

How Much Can We Learn from a Single Chromatographic Experiment? A Bayesian Perspective.

PubMed

Wiczling, Paweł; Kaliszan, Roman

2016-01-05

In this work, we proposed and investigated a Bayesian inference procedure to find the desired chromatographic conditions based on known analyte properties (lipophilicity, pKa, and polar surface area) using one preliminary experiment. A previously developed nonlinear mixed effect model was used to specify the prior information about a new analyte with known physicochemical properties. Further, the prior (no preliminary data) and posterior predictive distribution (prior + one experiment) were determined sequentially to search towards the desired separation. The following isocratic high-performance reversed-phase liquid chromatographic conditions were sought: (1) retention time of a single analyte within the range of 4-6 min and (2) baseline separation of two analytes with retention times within the range of 4-10 min. The empirical posterior Bayesian distribution of parameters was estimated using the "slice sampling" Markov Chain Monte Carlo (MCMC) algorithm implemented in Matlab. The simulations with artificial analytes and experimental data of ketoprofen and papaverine were used to test the proposed methodology. The simulation experiment showed that for a single and two randomly selected analytes, there is 97% and 74% probability of obtaining a successful chromatogram using none or one preliminary experiment. The desired separation for ketoprofen and papaverine was established based on a single experiment. It was confirmed that the search for a desired separation rarely requires a large number of chromatographic analyses at least for a simple optimization problem. The proposed Bayesian-based optimization scheme is a powerful method of finding a desired chromatographic separation based on a small number of preliminary experiments.

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

PubMed

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.

Inhibitory effect on in vitro LDL oxidation and HMG Co-A reductase activity of the liquid-liquid partitioned fractions of Hericium erinaceus (Bull.) Persoon (lion's mane mushroom).

PubMed

Rahman, Mohammad Azizur; Abdullah, Noorlidah; Aminudin, Norhaniza

2014-01-01

Oxidation of low-density lipoprotein (LDL) has been strongly suggested as the key factor in the pathogenesis of atherosclerosis. Mushrooms have been implicated in having preventive effects against chronic diseases due especially to their antioxidant properties. In this study, in vitro inhibitory effect of Hericium erinaceus on LDL oxidation and the activity of the cholesterol biosynthetic key enzyme, 3-hydroxy-3-methyl glutaryl coenzyme A (HMG Co-A) reductase, was evaluated using five liquid-liquid solvent fractions consisting of methanol : dichloromethane (M : DCM), hexane (HEX), dichloromethane (DCM), ethyl acetate (EA), and aqueous residue (AQ). The hexane fraction showed the highest inhibition of oxidation of human LDL as reflected by the increased lag time (100 mins) for the formation of conjugated diene (CD) at 1 µg/mL and decreased production (68.28%, IC50 0.73 mg/mL) of thiobarbituric acid reactive substances (TBARS) at 1 mg/mL. It also mostly inhibited (59.91%) the activity of the HMG Co-A reductase at 10 mg/mL. The GC-MS profiling of the hexane fraction identified the presence of myconutrients: inter alia, ergosterol and linoleic acid. Thus, hexane fraction of Hericium erinaceus was found to be the most potent in vitro inhibitor of both LDL oxidation and HMG Co-A reductase activity having therapeutic potential for the prevention of oxidative stress-mediated vascular diseases.

40 CFR 1065.267 - Gas chromatograph.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas chromatograph...

40 CFR 1065.267 - Gas chromatograph.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 33 2011-07-01 2011-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas chromatograph...

Bio-oil fractionation and condensation

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

Brown, Robert C.; Jones, Samuel T.; Pollard, Anthony

The present invention relates to a method of fractionating bio-oil vapors which involves providing bio-oil vapors comprising bio-oil constituents. The bio-oil vapors are cooled in a first stage which comprises a condenser having passages for the bio-oil separated by a heat conducting wall from passages for a coolant. The coolant in the condenser of the first stage is maintained at a substantially constant temperature, set at a temperature in the range of 75 to 100.degree. C., to condense a first liquid fraction of liquefied bio-oil constituents in the condenser of the first stage. The first liquid fraction of liquified bio-oilmore » constituents from the condenser in the first stage is collected. Also disclosed are steps for subsequently recovering further liquid fractions of liquefied bio-oil constituents. Particular compositions of bio-oil condensation products are also described.« less

Synthesis, fractionation, and thin film processing of nanoparticles using the tunable solvent properties of carbon dioxide gas expanded liquids

NASA Astrophysics Data System (ADS)

Anand, Madhu

Nanoparticles have received significant attention because of their unusual characteristics including high surface area to volume ratios. Materials built from nanoparticles possess unique chemical, physical, mechanical and optical properties. Due to these properties, they hold potential in application areas such as catalysts, sensors, semiconductors and optics. At the same time, CO 2 in the form of supercritical fluid or CO2 gas-expanded liquid mixtures has gained significant attention in the area of processing nanostructures. This dissertation focuses on the synthesis and processing of nanoparticles using CO2 tunable solvent systems. Nanoparticle properties depend heavily on their size and, as such, the ability to finely control the size and uniformity of nanoparticles is of utmost importance. Solution based nanoparticle formation techniques are attractive due to their simplicity, but they often result in the synthesis of particles with a wide size range. To address this limitation, a post-synthesis technique has been developed in this dissertation to fractionate polydisperse nanoparticles ( s . = 30%) into monodisperse fractions ( s . = 8%) using tunable physicochemical properties of CO 2 expanded liquids, where CO2 is employed as an antisolvent. This work demonstrates that by controlling the addition of CO2 (pressurization) to an organic dispersion of nanoparticles, the ligand stabilized nanoparticles can be size selectively precipitated within a novel high pressure apparatus that confines the particle precipitation to a specified location on a surface. Unlike current techniques, this CO2 expanded liquid approach provides faster and more efficient particle size separation, reduction in organic solvent usage, and pressure tunable size selection in a single process. To improve our fundamental understanding and to further refine the size separation process, a detailed study has been performed to identify the key parameters enabling size separation of various

Identification and measurement of beta-lactam antibiotic residues in milk: integration of screening kits with liquid chromatography.

PubMed

Harik-Khan, R; Moats, W A

1995-01-01

A procedure for identifying and quantitating violative beta-lactams in milk is described. This procedure integrates beta-lactam residue detection kits with the multiresidue automated liquid chromatographic (LC) cleanup method developed in our laboratory. Spiked milk was deproteinized, extracted, and subjected to reversed-phase LC using a gradient program that concentrated the beta-lactams. Amoxicillin, ampicillin, cephapirin, ceftiofur, cloxacillin, and penicillin G were, thus, separated into 5 fractions that were subsequently tested for activity by using 4 kits. beta-lactams in the positive fractions were quantitated by analytical LC methods developed in our laboratory. The LC cleanup method separated beta-lactam antibiotics from each other and from interferences in the matrix and also concentrated the antibiotics, thus increasing the sensitivity of the kits to the beta-lactam antibiotics. The procedure facilitated the task of identifying and measuring the beta-lactam antibiotics that may be present in milk samples.

Rapid Isocratic Liquid Chromatographic Separation and Quantification of Tryptophan and Six kynurenine Metabolites in Biological Samples with Ultraviolet and Fluorimetric Detection

PubMed Central

Badawy, Abdulla A-B; Morgan, Christopher J

2010-01-01

A simple, rapid isocratic liquid chromatographic procedure with ultraviolet and fluorimetric detection is described for the separation and quantification of L-tryptophan (Trp) and six of its kynurenine metabolites (kynurenine, 3-hydroxykynurenine, and 3-hydroxyanthranilic, kynurenic, xanthurenic and anthranilic acids). Using the Perkin Elmer LC 200 system, a reverse phase Synergi 4 μ fusion-RP80 A column (250 × 4.6 mm) (Phenomenex), and a mobile phase of 10 mM sodium dihydrogen phosphate: methanol (73:27, by vol) at pH 2.8 and a flow rate of 1.0–1.2 ml/min at 37 °C, a run took ∼13 min. The run took <7 min at 40 °C and a 1.4 ml/min flow rate. Limits of detection of all 7 analytes were 5–72 nM and their recoveries from human plasma and rat serum and liver varied between 62% and 111%. This simple method is suitable for high throughput work and can be further developed to include quinolinic acid and other Trp metabolites. PMID:22084598

High-performance liquid chromatographic method for profiling 2-oxo acids in urine and its application in evaluating vitamin status in rats.

PubMed

Shibata, Katsumi; Nakata, Chifumi; Fukuwatari, Tsutomu

2016-01-01

B-group vitamins are involved in the catabolism of 2-oxo acids. To identify the functional biomarkers of B-group vitamins, we developed a high-performance liquid chromatographic method for profiling 2-oxo acids in urine and applied this method to urine samples from rats deficient in vitamins B1 and B6 and pantothenic acid. 2-Oxo acids were reacted with 1,2-diamino-4,5-methylenebenzene to produce fluorescent derivatives, which were then separated using a TSKgel ODS-80Ts column with 30 mmol/L of KH2PO4 (pH 3.0):acetonitrile (7:3) at a flow rate of 1.0 mL/min. Vitamin B1 deficiency increased urinary levels of all 2-oxo acids, while vitamin B6 deficiency only increased levels of sum of 2-oxaloacetic acid and pyruvic acid, and pantothenic acid deficiency only increased levels of 2-oxoisovaleric acid. Profiles of 2-oxo acids in urine samples might be a non-invasive way of clarifying the functional biomarker of B-group vitamins.

Field-flow fractionation of nano- and microparticles in rotating coiled columns.

PubMed

Fedotov, Petr S; Ermolin, Mikhail S; Katasonova, Olesya N

2015-02-13

Field-flow fractionation (FFF) is a very powerful and versatile set of liquid chromatography-like elution methods. However, conventional FFF separations occur in thin channels and the sample weight injected is usually less than 1 mg to avoid overloading. The fractionation in a rotating coiled column (RCC), which can be attributed to sedimentation FFF, enables the handling sample weight to be increased at least up to 1 g. An uneven distribution of particles in RCC was first observed by Y. Ito et al. in 1966. The work in this direction was continued by P.S. Fedotov et al. in 2000. Regularities of the behaviour of nano- and microparticles of different size and origin in RCCs with different design parameters were systematically studied taking as example silica particles, latex beads, quartz sand, clay minerals, and other samples. The basic principles of the new FFF method were established. The developed method was applied to the speciation analysis of polydisperse environmental samples, in particular, for the separation of soils into silt, clay and sand fractions. For the first time, nano- and submicron particles of street dust have been separated, weighted, characterized by electronic microscopy, and quantitatively analyzed by ICP-MS (after digestion). The elements that may be of anthropogenic origin (Zn, Cr, Ni, Cu, Cd, Sn, Pb) were found to concentrate mainly in <0.3 and 0.3-1 μm fractions. It has been shown that the concentrations of Cr, Ni, Zn in the finest fraction (<0.3 μm) of street dust can be one order of magnitude higher than the concentrations of elements in bulk sample. The fractionation in RCC was also used for the recovery of a nearly monodisperse fraction (4.5 μm) of a chromatographic sorbent based on polystyrene-divinylbenzene; impurities remaining from the synthesis and smaller particles (1-2 μm) being removed. Study on the fractionation of synthetic samples has demonstrated the applicability of the method to the preparative separation and

A bridging study for oxytetracycline in the edible fillet of rainbow trout: Analysis by a liquid chromatographic method and the official microbial inhibition assay

USGS Publications Warehouse

Stehly, G.R.; Gingerich, W.H.; Kiessling, C.R.; Cutting, J.H.

1999-01-01

Oxytetracycline (OTC) is a drug approved by the U.S. Food and Drug Administration (FDA) to control certain diseases in salmonids and catfish. OTC is also a likely control agent for diseases of other fish species and for other diseases of salmonids and catfish not currently on the label. One requirement for FDA to extend and expand the approval of this antibacterial agent to other fish species is residue depletion studies. The current regulatory method for OTC in fish tissue, based on microbial inhibition, lacks sensitivity and specificity. To conduct residue depletion studies for OTC in fish with a liquid chromatographic method, a bridging study was required to determine its relationship with the official microbial inhibition assay. Triplicate samples of rainbow trout fillet tissue fortified with OTC at 0.3, 0.6, 1.2, 2.4, 4.8, and 9.6 ppm and fillet tissue with incurred OTC at approximately 0.75, 1.5, and 3.75 ppm were analyzed by high-performance liquid chromatography (HPLC) and the microbial inhibition assay. The results indicated that the 2 methods are essentially identical in the tested range, with mean coefficients of variation of 1.05% for the HPLC method and 3.94% for the microbial inhibition assay.

Advances in native high-performance liquid chromatography and intact mass spectrometry for the characterization of biopharmaceutical products.

PubMed

Tassi, Marco; De Vos, Jelle; Chatterjee, Sneha; Sobott, Frank; Bones, Jonathan; Eeltink, Sebastiaan

2018-01-01

The characterization of biotherapeutics represents a major analytical challenge. This review discusses the current state-of-the-art in analytical technologies to profile biopharma products under native conditions, i.e., the protein three dimensional conformation is maintained during liquid chromatographic analysis. Native liquid-chromatographic modes that are discussed include aqueous size-exclusion chromatography, hydrophobic interaction chromatography, and ion-exchange chromatography. Infusion conditions and the possibilities and limitations to hyphenate native liquid chromatography to mass spectrometry are discussed. Furthermore, the applicability of native liquid-chromatography methods and intact mass spectrometry analysis for the characterization of monoclonal antibodies and antibody-drug conjugates is discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dynamic heterogeneity in crossover spin facilitated model of supercooled liquid and fractional Stokes-Einstein relation

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

Choi, Seo-Woo; Kim, Soree; Jung, YounJoon, E-mail: yjjung@snu.ac.kr

Kinetically constrained models have gained much interest as models that assign the origins of interesting dynamic properties of supercooled liquids to dynamical facilitation mechanisms that have been revealed in many experiments and numerical simulations. In this work, we investigate the dynamic heterogeneity in the fragile-to-strong liquid via Monte Carlo method using the model that linearly interpolates between the strong liquid-like behavior and the fragile liquid-like behavior by an asymmetry parameter b. When the asymmetry parameter is sufficiently small, smooth fragile-to-strong transition is observed both in the relaxation time and the diffusion constant. Using these physical quantities, we investigate fractional Stokes-Einsteinmore » relations observed in this model. When b is fixed, the system shows constant power law exponent under the temperature change, and the exponent has the value between that of the Frederickson-Andersen model and the East model. Furthermore, we investigate the dynamic length scale of our systems and also find the crossover relation between the relaxation time. We ascribe the competition between energetically favored symmetric relaxation mechanism and entropically favored asymmetric relaxation mechanism to the fragile-to-strong crossover behavior.« less

Quantitative ionspray liquid chromatographic/tandem mass spectrometric determination of reserpine in equine plasma.

PubMed

Anderson, M A; Wachs, T; Henion, J D

1997-02-01

A method based on ionspray liquid chromatography/tandem mass spectrometry (LC/MS/MS) was developed for the determination of reserpine in equine plasma. A comparison was made of the isolation of reserpine from plasma by liquid-liquid extraction and by solid-phase extraction. A structural analog, rescinnamine, was used as the internal standard. The reconstituted extracts were analyzed by ionspray LC/MS/MS in the selected reaction monitoring (SRM) mode. The calibration graph for reserpine extracted from equine plasma obtained using liquid-liquid extraction was linear from 10 to 5000 pg ml-1 and that using solid-phase extraction from 100 to 5000 pg ml-1. The lower level of quantitation (LLQ) using liquid-liquid and solid-phase extraction was 50 and 200 pg ml-1, respectively. The lower level of detection for reserpine by LC/MS/MS was 10 pg ml-1. The intra-assay accuracy did not exceed 13% for liquid-liquid and 12% for solid-phase extraction. The recoveries for the LLQ were 68% for liquid-liquid and 58% for solid-phase extraction.

Portable gas chromatograph-mass spectrometer

DOEpatents

Andresen, B.D.; Eckels, J.D.; Kimmons, J.F.; Myers, D.W.

1996-06-11

A gas chromatograph-mass spectrometer (GC-MS) is described for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units. 4 figs.

Portable gas chromatograph-mass spectrometer

DOEpatents

Andresen, Brian D.; Eckels, Joel D.; Kimmons, James F.; Myers, David W.

1996-01-01

A gas chromatograph-mass spectrometer (GC-MS) for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units.

Characterization of multiblock copolymers by chromatographic techniques.

PubMed

N'Goma, Patrick Yoba; Radke, Wolfgang; Malz, Frank; Ziegler, Hans Jörg; Zierke, Michael; Behl, Marc; Lendlein, Andreas

2011-02-01

Multiblock copolymers (MBC) composed of blocks of poly(1,4-dioxanone) (PPDO) and poly(e-caprolactone) (PCL) were investigated in order to gain information on the extend of chemical heterogeneity of the samples. A gradient chromatographic method was established allowing separation of purely PPDO- from purely PCL-containing chains. Application of the gradient to MBC made of PPDO- and PCL-diols connected by trimethylhexamethylene diisocyanate (TMDI) resulted in two well separated peaks which were analyzed by means of FTIR, 1H-NMR and pyrolysis GC-MS. It was shown that the first peak was composed to a large extent of PPDO and only lower amounts of PCL were incorporated. Conversely, the second peak consisted predominantly of PCL with only a minor fraction of PPDO. Thus, the MBCs having PPDO and PCL segments show an unexpected broad chemical heterogeneity.

APPLICATION OF A SPRAY DEPOSITION METHOD FOR REVERSED PHASE LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

EPA Science Inventory

Four coal gasification wastewater samples were analyzed for nonvolatile and polar organics by liquid chromatography-mass spectrometry (LC/MS). Samples were separated on a reverse phase liquid chromatographic column using an aqueous solvent as the eluant. A special spray depositio...

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

PubMed

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

2015-08-28

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

Inhibitory Effect on In Vitro LDL Oxidation and HMG Co-A Reductase Activity of the Liquid-Liquid Partitioned Fractions of Hericium erinaceus (Bull.) Persoon (Lion's Mane Mushroom)

PubMed Central

Aminudin, Norhaniza

2014-01-01

Oxidation of low-density lipoprotein (LDL) has been strongly suggested as the key factor in the pathogenesis of atherosclerosis. Mushrooms have been implicated in having preventive effects against chronic diseases due especially to their antioxidant properties. In this study, in vitro inhibitory effect of Hericium erinaceus on LDL oxidation and the activity of the cholesterol biosynthetic key enzyme, 3-hydroxy-3-methyl glutaryl coenzyme A (HMG Co-A) reductase, was evaluated using five liquid-liquid solvent fractions consisting of methanol : dichloromethane (M : DCM), hexane (HEX), dichloromethane (DCM), ethyl acetate (EA), and aqueous residue (AQ). The hexane fraction showed the highest inhibition of oxidation of human LDL as reflected by the increased lag time (100 mins) for the formation of conjugated diene (CD) at 1 µg/mL and decreased production (68.28%, IC50 0.73 mg/mL) of thiobarbituric acid reactive substances (TBARS) at 1 mg/mL. It also mostly inhibited (59.91%) the activity of the HMG Co-A reductase at 10 mg/mL. The GC-MS profiling of the hexane fraction identified the presence of myconutrients: inter alia, ergosterol and linoleic acid. Thus, hexane fraction of Hericium erinaceus was found to be the most potent in vitro inhibitor of both LDL oxidation and HMG Co-A reductase activity having therapeutic potential for the prevention of oxidative stress-mediated vascular diseases. PMID:24959591

Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

PubMed

Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

2014-01-01

Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

Identification and phylogeny of Arabian snakes: Comparison of venom chromatographic profiles versus 16S rRNA gene sequences.

PubMed

Al Asmari, Abdulrahman; Manthiri, Rajamohammed Abbas; Khan, Haseeb Ahmad

2014-11-01

Identification of snake species is important for various reasons including the emergency treatment of snake bite victims. We present a simple method for identification of six snake species using the gel filtration chromatographic profiles of their venoms. The venoms of Echis coloratus, Echis pyramidum, Cerastes gasperettii, Bitis arietans, Naja arabica, and Walterinnesia aegyptia were milked, lyophilized, diluted and centrifuged to separate the mucus from the venom. The clear supernatants were filtered and chromatographed on fast protein liquid chromatography (FPLC). We obtained the 16S rRNA gene sequences of the above species and performed phylogenetic analysis using the neighbor-joining method. The chromatograms of venoms from different snake species showed peculiar patterns based on the number and location of peaks. The dendrograms generated from similarity matrix based on the presence/absence of particular chromatographic peaks clearly differentiated Elapids from Viperids. Molecular cladistics using 16S rRNA gene sequences resulted in jumping clades while separating the members of these two families. These findings suggest that chromatographic profiles of snake venoms may provide a simple and reproducible chemical fingerprinting method for quick identification of snake species. However, the validation of this methodology requires further studies on large number of specimens from within and across species.

Estimation of descriptors for hydrogen-bonding compounds from chromatographic and liquid-liquid partition measurements.

PubMed

Lenca, Nicole; Atapattu, Sanka N; Poole, Colin F

2017-12-01

Retention factors obtained by gas chromatography and reversed-phase liquid chromatography on varied columns and partition constants in different liquid-liquid partition systems are used to estimate WSU descriptor values for 36 anilines and N-heterocyclic compounds, 13 amides and related compounds, and 45 phenols and alcohols. These compounds are suitable for use as calibration compounds to characterize separation systems covering the descriptor space E=0.2-3, S=0.4-2.1, A=0-1.5, B=0.1-1.5, L=2.5-10.0 and V=0.5-2.2. Hydrogen-bonding properties are discussed in terms of structure, the possibility of induction effects, intramolecular hydrogen bonding and steric factors for anilines, amides, phenols and alcohols. The relationship between these parameters and observed descriptor values are difficult to predict from structure but facilitate improving the general occupancy of the descriptor space by creating incremental changes in hydrogen-bonding properties. It is verified that the compounds included in this study can be merged with an existing database of compounds recommended for characterizing separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

Chromatographic hydrogen isotope separation

DOEpatents

Aldridge, Frederick T.

1981-01-01

Intermetallic compounds with the CaCu.sub.5 type of crystal structure, particularly LaNiCo.sub.4 and CaNi.sub.5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors.

Chromatographic hydrogen isotope separation

DOEpatents

Aldridge, F.T.

Intermetallic compounds with the CaCu/sub 5/ type of crystal structure, particularly LaNiCo/sub 4/ and CaNi/sub 5/, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen cn produce large quantities of heavy water at an effective cost for use in heavy water reactors.

Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

PubMed

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.

Fuels characterization studies. [jet fuels

NASA Technical Reports Server (NTRS)

Seng, G. T.; Antoine, A. C.; Flores, F. J.

1980-01-01

Current analytical techniques used in the characterization of broadened properties fuels are briefly described. Included are liquid chromatography, gas chromatography, and nuclear magnetic resonance spectroscopy. High performance liquid chromatographic ground-type methods development is being approached from several directions, including aromatic fraction standards development and the elimination of standards through removal or partial removal of the alkene and aromatic fractions or through the use of whole fuel refractive index values. More sensitive methods for alkene determinations using an ultraviolet-visible detector are also being pursued. Some of the more successful gas chromatographic physical property determinations for petroleum derived fuels are the distillation curve (simulated distillation), heat of combustion, hydrogen content, API gravity, viscosity, flash point, and (to a lesser extent) freezing point.

A Small-Scale Low-Cost Gas Chromatograph

ERIC Educational Resources Information Center

Gros, Natasa; Vrtacnik, Margareta

2005-01-01

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

Semi-micro high-performance liquid chromatographic analysis of tiropramide in human plasma using column-switching.

PubMed

Baek, Soo Kyoung; Lee, Seung Seok; Park, Eun Jeon; Sohn, Dong Hwan; Lee, Hye Suk

2003-02-05

A rapid and sensitive column-switching semi-micro high-performance liquid chromatography method was developed for the direct analysis of tiropramide in human plasma. The plasma sample (100 microl) was directly injected onto Capcell Pak MF Ph-1 precolumn where deproteinization and analyte fractionation occurred. Tiropramide was then eluted into an enrichment column (Capcell Pak UG C(18)) using acetonitrile-potassium phosphate (pH 7.0, 50 mM) (12:88, v/v) and was analyzed on a semi-micro C(18) analytical column using acetonitrile-potassium phosphate (pH 7.0, 10 mM) (50:50, v/v). The method showed excellent sensitivity (limit of quantification 5 ng/ml), and good precision (C.V.

Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

PubMed

Sun, Jianghao; Chen, Pei

2012-03-05

A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims. Copyright © 2011. Published by Elsevier B.V.

On-line coupling of supercritical fluid extraction and chromatographic techniques.

PubMed

Sánchez-Camargo, Andrea Del Pilar; Parada-Alfonso, Fabián; Ibáñez, Elena; Cifuentes, Alejandro

2017-01-01

This review summarizes and discusses recent advances and applications of on-line supercritical fluid extraction coupled to liquid chromatography, gas chromatography, and supercritical fluid chromatographic techniques. Supercritical fluids, due to their exceptional physical properties, provide unique opportunities not only during the extraction step but also in the separation process. Although supercritical fluid extraction is especially suitable for recovery of non-polar organic compounds, this technique can also be successfully applied to the extraction of polar analytes by the aid of modifiers. Supercritical fluid extraction process can be performed following "off-line" or "on-line" approaches and their main features are contrasted herein. Besides, the parameters affecting the supercritical fluid extraction process are explained and a "decision tree" is for the first time presented in this review work as a guide tool for method development. The general principles (instrumental and methodological) of the different on-line couplings of supercritical fluid extraction with chromatographic techniques are described. Advantages and shortcomings of supercritical fluid extraction as hyphenated technique are discussed. Besides, an update of the most recent applications (from 2005 up to now) of the mentioned couplings is also presented in this review. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent advances of ionic liquids and polymeric ionic liquids in capillary electrophoresis and capillary electrochromatography.

PubMed

Tang, Sheng; Liu, Shujuan; Guo, Yong; Liu, Xia; Jiang, Shengxiang

2014-08-29

Ionic liquids (ILs) and polymeric ionic liquids (PILs) with unique and fascinating properties have drawn considerable interest for their use in separation science, especially in chromatographic techniques. In this article, significant contributions of ILs and PILs in the improvement of capillary electrophoresis and capillary electrochromatography are described, and a specific overview of the most relevant examples of their applications in the last five years is also given. Accordingly, some general conclusions and future perspectives in these areas are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2013-02-01

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

Multichannel Detection in High-Performance Liquid Chromatography.

ERIC Educational Resources Information Center

Miller, James C.; And Others

1982-01-01

A linear photodiode array is used as the photodetector element in a new ultraviolet-visible detection system for high-performance liquid chromatography (HPLC). Using a computer network, the system processes eight different chromatographic signals simultaneously in real-time and acquires spectra manually/automatically. Applications in fast HPLC…

Predicting drug penetration across the blood-brain barrier: comparison of micellar liquid chromatography and immobilized artificial membrane liquid chromatography.

PubMed

De Vrieze, Mike; Lynen, Frédéric; Chen, Kai; Szucs, Roman; Sandra, Pat

2013-07-01

Several in vitro methods have been tested for their ability to predict drug penetration across the blood-brain barrier (BBB) into the central nervous system (CNS). In this article, the performance of a variety of micellar liquid chromatographic (MLC) methods and immobilized artificial membrane (IAM) liquid chromatographic approaches were compared for a set of 45 solutes. MLC measurements were performed on a C18 column with sodium dodecyl sulfate (SDS), polyoxyethylene (23) lauryl ether (Brij35), or sodium deoxycholate (SDC) as surfactant in the micellar mobile phase. IAM liquid chromatography measurements were performed with Dulbecco's phosphate-buffered saline (DPBS) and methanol as organic modifier in the mobile phase. The corresponding retention and computed descriptor data for each solute were used for construction of models to predict transport across the blood-brain barrier (log BB). All data were correlated with experimental log BB values and the relative performance of the models was studied. SDS-based models proved most suitable for prediction of log BB values, followed closely by a simplified IAM method, in which it could be observed that extrapolation of retention data to 0% modifier in the mobile phase was unnecessary.

Theory of Random Copolymer Fractionation in Columns

NASA Astrophysics Data System (ADS)

Enders, Sabine

Random copolymers show polydispersity both with respect to molecular weight and with respect to chemical composition, where the physical and chemical properties depend on both polydispersities. For special applications, the two-dimensional distribution function must adjusted to the application purpose. The adjustment can be achieved by polymer fractionation. From the thermodynamic point of view, the distribution function can be adjusted by the successive establishment of liquid-liquid equilibria (LLE) for suitable solutions of the polymer to be fractionated. The fractionation column is divided into theoretical stages. Assuming an LLE on each theoretical stage, the polymer fractionation can be modeled using phase equilibrium thermodynamics. As examples, simulations of stepwise fractionation in one direction, cross-fractionation in two directions, and two different column fractionations (Baker-Williams fractionation and continuous polymer fractionation) have been investigated. The simulation delivers the distribution according the molecular weight and chemical composition in every obtained fraction, depending on the operative properties, and is able to optimize the fractionation effectively.

Microbial communities in liquid and fiber fractions of food waste digestates are differentially resistant to inhibition by ammonia.

PubMed

Peng, Wei; Lü, Fan; Shao, Liming; He, Pinjing

2015-04-01

The effect of different concentrations of ammonia (1.0-7.0 g/L) during mesophilic anaerobic digestion with fiber or liquid digestate as inoculum was examined. Evolution of microbial community within fiber and liquid digestates was quantitatively assessed by the intact lipid analysis methods and qualitatively by DNA fingerprint methods in order to determine their resistance to ammonia inhibition. The results showed that an increased level of total ammonia nitrogen prolonged the lag phase of fiber digestates while reduced the metabolic rate of liquid digestates. Fiber digestates had 19.6-50.9-fold higher concentrations of phospholipid fatty acids (PLFA) compared to liquid digestates, whereas concentrations of phospholipid ether lipids (PLEL) in the fiber digestates were only 2.91-17.6-fold higher compared to liquid digestates. Although the cell concentration in liquid fraction was far lower than that in the fiber one, the ammonia-resistant ability and the methanization efficiency of the liquid digestate was superior to the fiber digestate. The bacterial profiles were affected more by the type of digestate inoculum compared to the concentration of ammonia. Principal component analysis indicated that the lipids technique was superior to the DNA technique for bacterial quantification but detected less archaeal diversity.

[Advances of poly (ionic liquid) materials in separation science].

PubMed

Liu, Cuicui; Guo, Ting; Su, Rina; Gu, Yuchen; Deng, Qiliang

2015-11-01

Ionic liquids, as novel ionization reagents, possess beneficial characteristics including good solubility, conductivity, thermal stability, biocompatibility, low volatility and non-flammability. Ionic liquids are attracting a mass of attention of analytical chemists. Poly (ionic liquid) materials have common performances of ionic liquids and polymers, and have been successfully applied in separation science area. In this paper, we discuss the interaction mechanisms between the poly(ionic liquid) materials and analytes including hydrophobic/hydrophilic interactions, hydrogen bond, ion exchange, π-π stacking and electrostatic interactions, and summarize the application advances of the poly(ionic liquid) materials in solid phase extraction, chromatographic separation and capillary electrophoresis. At last, we describe the future prospect of poly(ionic liquid) materials.

Determination of teicoplanin concentrations in serum by high-pressure liquid chromatography.

PubMed Central

Joos, B; Lüthy, R

1987-01-01

An isocratic reversed-phase high-pressure liquid chromatographic method for the determination of six components of the teicoplanin complex in biological fluid was developed. By using fluorescence detection after precolumn derivatization with fluorescamine, the assay is specific and highly sensitive, with reproducibility studies yielding coefficients of variation ranging from 1.5 to 8.5% (at 5 to 80 micrograms/ml). Response was linear from 2.5 to 80 micrograms/ml (r = 0.999); the recovery from spiked human serum was 76%. An external quality control was performed to compare this high-pressure liquid chromatographic method (H) with a standard microbiological assay (M); no significant deviation from slope = 1 and intercept = 0 was found by regression analysis (H = 1.03M - 0.45; n = 15). PMID:2957953

Gaining insight in the behaviour of imidazolium-based ionic liquids as additives in reversed-phase liquid chromatography for the analysis of basic compounds.

PubMed

Ubeda-Torres, M T; Ortiz-Bolsico, C; García-Alvarez-Coque, M C; Ruiz-Angel, M J

2015-02-06

In reversed-phase liquid chromatography in the absence of additives, cationic basic compounds give rise to broad and asymmetrical peaks as a result of ionic interactions with residual free silanols on silica-based stationary phases. Ionic liquids (ILs), added to the mobile phase, have been suggested as alternatives to amines to block the activity of silanols. However, the dual character of ILs should be considered: both cation and anion may be adsorbed on the stationary phase, thereby creating a double asymmetrical layer positively or negatively charged, depending on the relative adsorption of both ions. In this work, a study of the performance of six imidazolium-based ILs (the chlorides and tetrafluoroborates of 1-ethyl-, 1-butyl- and 1-hexyl-3-methylimidazolium) as modifiers of the chromatographic behaviour of a group of 10 β-blockers is performed, and compared with triethylamine and dimethyloctylamine. In order to gain more insight in the behaviour of ILs in RPLC, the changes in the nature of the chromatographic system, at increasing concentration of the additives, were followed based on retention and peak shape modelling. The multiple interactions that amines and ILs experience inside the chromatographic system suggest that the suppressing potency should be measured based on the shape of chromatographic peaks and not on the changes in retention. The ILs 1-hexyl-3-methyl-imidazolium chloride and tetrafluoroborate offered the most interesting features for the separation of the basic drugs. Copyright © 2014 Elsevier B.V. All rights reserved.

Solid-phase extraction NMR studies of chromatographic fractions of saponins from Quillaja saponaria.

PubMed

Nyberg, Nils T; Baumann, Herbert; Kenne, Lennart

2003-01-15

The saponin mixture QH-B from the tree Quillaja saponaria var. Molina was fractionated by RP-HPLC in several steps. The fractions were analyzed by solid-phase extraction NMR (SPE-NMR), a technique combining the workup by solid-phase extraction with on-line coupling to an NMR flow probe. Together with MALDI-TOF mass spectrometry and comparison with chemical shifts of similar saponins, the structures of both major and minor components in QH-B could be obtained. The procedure described is a simple method to determine the structure of components in a complex mixture. The two major fractions of the mixture were found to contain at least 28 saponins, differing in the carbohydrate substructures. Eight of these have not previously been determined. The 28 saponins formed 14 equilibrium pairs by the migration of an O-acyl group between two adjacent positions on a fucosyl residue.

Fluorescence-correlation spectroscopy study of molecular transport within reversed-phase chromatographic particles compared to planar model surfaces.

PubMed

Cooper, Justin; Harris, Joel M

2014-12-02

Reversed-phase liquid chromatography (RPLC) is a widely used technique for molecular separations. Stationary-phase materials for RPLC generally consist of porous silica-gel particles functionalized with n-alkane ligands. Understanding motions of molecules within the interior of these particles is important for developing efficient chromatographic materials and separations. To characterize these dynamics, time-resolved spectroscopic methods (photobleach recovery, fluorescence correlation, single-molecule imaging) have been adapted to measure molecular diffusion rates, typically at n-alkane-modified planar silica surfaces, which serve as models of chromatographic interfaces. A question arising from these studies is how dynamics of molecules on a planar surface relate to motions of molecules within the interior of a porous chromatographic particle. In this paper, imaging-fluorescence-correlation spectroscopy is used to measure diffusion rates of a fluorescent probe molecule 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbocyanine perchlorate (DiI) within authentic RPLC porous silica particles and compared with its diffusion at a planar C18-modified surface. The results show that surface diffusion on the planar C18 substrate is much faster than the diffusion rate of the probe molecule through a chromatographic particle. Surface diffusion within porous particles, however, is governed by molecular trajectories along the tortuous contours of the interior surface of the particles. By accounting for the greater surface area that a molecule must explore to diffuse macroscopic distances through the particle, the molecular-scale diffusion rates on the two surfaces can be compared, and they are virtually identical. These results provide support for the relevance of surface-diffusion measurements made on planar model surfaces to the dynamic behavior of molecules on the internal surfaces of porous chromatographic particles.

Space Group Symmetry Fractionalization in a Chiral Kagome Heisenberg Antiferromagnet.

PubMed

Zaletel, Michael P; Zhu, Zhenyue; Lu, Yuan-Ming; Vishwanath, Ashvin; White, Steven R

2016-05-13

The anyonic excitations of a spin liquid can feature fractional quantum numbers under space group symmetries. Detecting these fractional quantum numbers, which are analogs of the fractional charge of Laughlin quasiparticles, may prove easier than the direct observation of anyonic braiding and statistics. Motivated by the recent numerical discovery of spin-liquid phases in the kagome Heisenberg antiferromagnet, we theoretically predict the pattern of space group symmetry fractionalization in the kagome lattice SO(3)-symmetric chiral spin liquid. We provide a method to detect these fractional quantum numbers in finite-size numerics which is simple to implement in the density matrix renormalization group. Applying these developments to the chiral spin liquid phase of a kagome Heisenberg model, we find perfect agreement between our theoretical prediction and numerical observations.

[UPLC characteristic chromatographic profile of Poria].

PubMed

Zhang, Qi; Wang, Zhenzhong; Xiao, Wei; Zhang, Liangqi; Bi, Kaishun; Jia, Ying

2012-04-01

To establish a UPLC characteristic chromatographic profile analysis method to quickly assess Poria quality and provide basis fro controlling Poria quality. The UPLC characteristic chromatographic profiles of fifteen batches of Poria were determined by ACQUITY UPLC, with HSS T3 Column (2.1 mm x 100 mm, 1.8 microm) eluted with the mobile phases of water containing 0.05% phosphoric acid and acetonitrile in gradient mode. The detection wavelength was set at 243 nm. The common mode of the UPLC characteristic chromatographic profile was set up. There were 20 common peaks, seven of which were identified, and the similar degrees of the fifteen samples to the common mode were between 0.787 and 0.974. The method was so time-saving that it can be used for the quality control of Poria.

Probabilistic peak detection for first-order chromatographic data.

PubMed

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

2014-03-19

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

Trapped Melt in IIIAB Irons: Solid/Liquid Elemental Partitioning During the Fractionation of the IIIAB Magma

NASA Technical Reports Server (NTRS)

Wasson, John T.

1999-01-01

Group IIIAB, the largest iron-meteorite group, shows compositional trends (including a three-order-of-magnitude It concentration range) indicating that it formed by fractional crystallization of a metallic magma. Because about 200 irons are available, and all degrees of crystallization are well represented, IIIAB offers an excellent set of samples for the study of crystallization at all depths of the asteroidal core. On log-log Ir-Au, and Ir-As diagrams IIIAB forms a broad band; the breadth represents real meteorite-to-meteorite variations, far outside experimental or sampling uncertainties. A successful model must explain the width of this band; I suggest that it mainly resulted from the trapping of parental magma within the crystallizing solid. Because S is essentially insoluble in metal, the abundance of FeS is a measure of the fraction of trapped liquid. The trapped-melt model is supported by the observation that irons having higher S contents plot closer to the inferred composition of the magmatic parental liquid. The lowest S values are found in the irons occupying the left envelope of the IIIAB Ir-Au or Ir-As compositional fields, thus it is this set of irons that should be interpreted as the solid products of a fractionating magma. This simplifies the modeling of the crystallization process and allows inferences regarding the distribution ratios for other elements in the evolved IIIAB system. The large (multiton) Cape York irons show wide variations in their trapped-melt fractions; their compositions seem best understood in terms of a low initial S content of the IIIAB magma, about 20 mg/g. The inferred initial IIIAB distribution coefficient for Ir, 4.6, is much higher than published values based on laboratory studies of low-S systems; I suggest that low-S (and low-P) partition-ratio measurements tend to err in the direction of unity. In IIIAB distribution coefficients for Au, As, and Ni were still < 1 when the most evolved IIIAB irons formed, another

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

PubMed

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

2008-01-01

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

Incorporating high-pressure electroosmotic pump and a nano-flow gradient generator into a miniaturized liquid chromatographic system for peptide analysis.

PubMed

Chen, Apeng; Lynch, Kyle B; Wang, Xiaochun; Lu, Joann J; Gu, Congying; Liu, Shaorong

2014-09-24

We integrate a high-pressure electroosmotic pump (EOP), a nanoflow gradient generator, and a capillary column into a miniaturized liquid chromatographic system that can be directly coupled with a mass spectrometer for proteomic analysis. We have recently developed a low-cost high-pressure EOP capable of generating pressure of tens of thousands psi, ideal for uses in miniaturized HPLC. The pump worked smoothly when it was used for isocratic elutions. When it was used for gradient elutions, generating reproducible gradient profiles was challenging; because the pump rate fluctuated when the pump was used to pump high-content organic solvents. This presents an issue for separating proteins/peptides since high-content organic solvents are often utilized. In this work, we solve this problem by incorporating our high-pressure EOP with a nano-flow gradient generator so that the EOP needs only to pump an aqueous solution. With this combination, we develop a capillary-based nano-HPLC system capable of performing nano-flow gradient elution; the pump rate is stable, and the gradient profiles are reproducible and can be conveniently tuned. To demonstrate its utility, we couple it with either a UV absorbance detector or a mass spectrometer for peptide separations. Copyright © 2014. Published by Elsevier B.V.

Gas-liquid chromatography in lunar organic analysis.

NASA Technical Reports Server (NTRS)

Gehrke, C. W.

1972-01-01

Gas-liquid chromatography (GLC) is a powerful and sensitive method for the separation and detection of organic compounds at nanogram levels. The primary requirement for successful analyses is that the compounds of interest must be volatile under the chromatographic conditions employed. Nonvolatile organic compounds must be converted to volatile derivatives prior to analysis. The derivatives of choice must be both amenable to chromatographic separation and be relatively stable. The condition of volatility necessitates the development of efficient derivatization reactions for important groups of compounds as amino acids, carbohydrates, nucleosides, etc. Trimethylsilylation and trifluoroacetylation represent specific areas of recent prominence. Some relevant practical aspects of GLC are discussed.

Optimization of a liquid chromatographic method for determination of malachite green and its metabolites in fish tissues

USGS Publications Warehouse

Plakas, S.M.; ELSaid, K.R.; Stehly, G.R.; Roybal, J.E.

1995-01-01

A liquid chromatographic (LC) method was adapted and optimized for the determination of malachite green and its metabolites in fish plasma and muscle, Residues in plasma were extracted with acetonitrile, the extract was evaporated to dryness, and residues were resolubilized for LC analysis, Residues in muscle were extracted with an acetonitrile-acetate buffer mixture, reextracted with acetonitrile, and partitioned into methylene chloride with final cleanup on alumina and propylsulfonic acid solid-phase extraction columns, Residue levels were determined by using an LC cyano column with a PbO2 postcolumn and visible detection (618 nm). Overall mean recoveries of parent malachite green (MG-C) and its major metabolite, leucomalachite green (MG-L), from plasma were 93 and 87%, respectively, at fortification levels ranging from 25 to 250 ppb, Overall mean recoveries of MG-C and MG-L from muscle were 85 and 95%, respectively, at fortification levels ranging from 5 to 100 ppb, Relative standard deviations (RSDs) of recoveries at all fortification levels ranged from 3.9 to 7.0% for plasma and from 2.1 to 5.2% for muscle, The method was applied to incurred residues in tissues sampled from catfish after waterborne exposure to [C-14]MG-C. Mean recoveries of total radioactive residues in plasma and muscle throughout the extraction and cleanup process were 88 and 87%, respectively, and corresponding RSDs for MG-C and MG-L were in the same range as those for fortified tissues, MG-L, was confirmed as the major metabolite of MG-C in catfish.

On the use of ionic liquids as mobile phase additives in high-performance liquid chromatography. A review.

PubMed

García-Alvarez-Coque, M C; Ruiz-Angel, M J; Berthod, A; Carda-Broch, S

2015-07-09

The popularity of ionic liquids (ILs) has grown during the last decades in several analytical separation techniques. Consequently, the number of reports devoted to the applications of ILs is still increasing. This review is focused on the use of ILs (mainly imidazolium-based associated to chloride and tetrafluoroborate) as mobile phase additives in high-performance liquid chromatography (HPLC). In this approach, ILs just function as salts, but keep several kinds of intermolecular interactions, which are useful for chromatographic separations. Both cation and anion can be adsorbed on the stationary phase, creating a bilayer. This gives rise to hydrophobic, electrostatic and other specific interactions with the stationary phase and solutes, which modify the retention behaviour and peak shape. This review updates the advances in this field, with emphasis on topics not always deeply considered in the literature, such as the mechanisms of retention, the estimation of the suppressing potency of silanols, modelling and optimisation of the chromatographic performance, and the comparison with other additives traditionally used to avoid the silanol problem. Copyright © 2015 Elsevier B.V. All rights reserved.

ANALYSIS OF SELECTED CHEMICAL GROUPS BY LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY

EPA Science Inventory

The use of the moving-belt liquid chromatographic interface in combination with mass spectrometry was evaluated for determining detection limits of selected members of various chemical classes. mong the chemical classes examined were benzidines, nitrosoamines, anilines, nitroarom...

Chromatographic Techniques for Rare Earth Elements Analysis

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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

PubMed

Lesellier, Eric; Tchapla, Alain

2005-12-23

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

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

PubMed

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

2013-12-18

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

Control of ice chromatographic retention mechanism by changing temperature and dopant concentration.

PubMed

Tasaki, Yuiko; Okada, Tetsuo

2011-12-15

A liquid phase coexists with solid water ice in a typical binary system, such as NaCl-water, in the temperature range between the freezing point and the eutectic point (t(eu)) of the system. In ice chromatography with salt-doped ice as the stationary phase, both solid and liquid phase can contribute to solute retention in different fashions; that is, the solid ice surface acts as an adsorbent, while a solute can be partitioned into the liquid phase. Thus, both adsorption and partition mechanisms can be utilized for ice chromatographic separation. An important feature in this approach is that the liquid phase volume can be varied by changing the temperature and the concentration of a salt incorporated into the ice stationary phase. Thus, we can control the relative contribution from the partition mechanism in the entire retention because the liquid phase volume can be estimated from the freezing depression curve. Separation selectivity can thereby be modified. The applicability of this concept has been confirmed for the solutes of different adsorption and partition abilities. The predicted retention based on thermodynamics basically agrees well with the corresponding experimental retention. However, one important inconsistency has been found. The calculation predicts a step-like discontinuity of the solute retention at t(eu) because the phase diagram suggests that the liquid phase abruptly appears at t(eu) when the temperature increases. In contrast, the corresponding experimental plots are continuous over the wider range including the subeutectic temperatures. This discrepancy is explained by the existence of the liquid phase below t(eu). A difference between predicted and measured retention factors allows the estimation of the volume of the subeutectic liquid phase.

Migration through soil of organic solutes in an oil-shale process water

USGS Publications Warehouse

Leenheer, J.A.; Stuber, H.A.

1981-01-01

The migration through soil of organic solutes in an oil-shale process water (retort water) was studied by using soil columns and analyzing leachates for various organic constituents. Retort water extracted significant quantities of organic anions leached from ammonium-saturated-soil organic matter, and a distilled-water rinse, which followed retort-water leaching, released additional organic acids from the soil. After being corrected for organic constitutents extracted from soil by retort water, dissolved-organic-carbon fractionation analyses of effluent fractions showed that the order of increasing affinity of six organic compound classes for the soil was as follows: hydrophilic neutrals nearly equal to hydrophilic acids, followed by the sequence of hydrophobic acids, hydrophilic bases, hydrophobic bases, and hydrophobic neutrals. Liquid-chromatographic analysis of the aromatic amines in the hydrophobic- and hydrophilic-base fractions showed that the relative order of the rates of migration through the soil column was the same as the order of migration on a reversed-phase, octadecylsilica liquid-chromatographic column.

Deconvolution of gas chromatographic data

NASA Technical Reports Server (NTRS)

Howard, S.; Rayborn, G. H.

1980-01-01

The use of deconvolution methods on gas chromatographic data to obtain an accurate determination of the relative amounts of each material present by mathematically separating the merged peaks is discussed. Data were obtained on a gas chromatograph with a flame ionization detector. Chromatograms of five xylenes with differing degrees of separation were generated by varying the column temperature at selected rates. The merged peaks were then successfully separated by deconvolution. The concept of function continuation in the frequency domain was introduced in striving to reach the theoretical limit of accuracy, but proved to be only partially successful.

Rapid and Convenient Separation of Chitooligosaccharides by Ion-Exchange Chromatography

NASA Astrophysics Data System (ADS)

Wu, Yuxiao; Lu, Wei-Peng; Wang, Jianing; Gao, Yunhua; Guo, Yanchuan

2017-12-01

Pervious methods for separation of highly purified chitooligosaccharides was time-consuming and labor-intensive, which limited the large-scale production. This study developed a convenient ion-exchange chromatography using the ÄKTA™ avant 150 chromatographic system. Five fractions were automatically collected under detecting the absorption at 210 nm. The fractions were analyzed by high-performance liquid chromatography. It proved that they primarily comprised chitobiose, chitotriose, chitotetraose, chitopentaose, and chitohexaose, respectively, with chromatographic purities over 90%. The separation process was rapid, convenient and could be monitored on-line, which would be benefit for the mass production of chitooligosaccharides.

Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

NASA Astrophysics Data System (ADS)

Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

2016-05-01

High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

Polar Aprotic Modifiers for Chromatographic Separation and Back-Exchange Reduction for Protein Hydrogen/Deuterium Exchange Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

NASA Astrophysics Data System (ADS)

Valeja, Santosh G.; Emmett, Mark R.; Marshall, Alan G.

2012-04-01

Hydrogen/deuterium exchange monitored by mass spectrometry is an important non-perturbing tool to study protein structure and protein-protein interactions. However, water in the reversed-phase liquid chromatography mobile phase leads to back-exchange of D for H during chromatographic separation of proteolytic peptides following H/D exchange, resulting in incorrect identification of fast-exchanging hydrogens as unexchanged hydrogens. Previously, fast high-performance liquid chromatography (HPLC) and supercritical fluid chromatography have been shown to decrease back-exchange. Here, we show that replacement of up to 40% of the water in the LC mobile phase by the modifiers, dimethylformamide (DMF) and N-methylpyrrolidone (NMP) (i.e., polar organic modifiers that lack rapid exchanging hydrogens), significantly reduces back-exchange. On-line LC micro-ESI FT-ICR MS resolves overlapped proteolytic peptide isotopic distributions, allowing for quantitative determination of the extent of back-exchange. The DMF modified solvent composition also improves chromatographic separation while reducing back-exchange relative to conventional solvent.

Position sensitive radioactivity detection for gas and liquid chromatography

DOEpatents

Cochran, Joseph L.; McCarthy, John F.; Palumbo, Anthony V.; Phelps, Tommy J.

2001-01-01

A method and apparatus are provided for the position sensitive detection of radioactivity in a fluid stream, particularly in the effluent fluid stream from a gas or liquid chromatographic instrument. The invention represents a significant advance in efficiency and cost reduction compared with current efforts.

Liquid chromatographic-tandem mass spectrometric method for the simultaneous determination of alkylphenols polyethoxylates, alkylphenoxy carboxylates and alkylphenols in wastewater and surface-water.

PubMed

Ciofi, L; Ancillotti, C; Chiuminatto, U; Fibbi, D; Checchini, L; Orlandini, S; Del Bubba, M

2014-10-03

Four different pellicular stationary phases (i.e. octadecylsilane, octasilane, Phenyl-Hexyl and pentafluorophenyl) were investigated for the chromatographic resolution of alkylphenols (APs), alkylphenols polyethoxylates (APnEOs) and alkylphenoxy carboxylates (APECs) using mixtures of water and organic solvents (i.e. methanol, acetonitrile and tetrahydrofuran) as eluents, in order to obtain their determination by a single LC-MS/MS run. In fact, alkylphenols and alkylphenoxy carboxylates must be analysed in negative ion mode, whereas alkylphenols polyethoxylates undergo ionisation only in positive ion mode, and therefore, two distinct LC-MS/MS analysis are commonly adopted. The best resolution among the aforementioned target analytes was achieved on the pentafluorophenyl column, eluting with an acidified water-acetonitrile-tetrahydrofuran mixture and using the post column addition of an ammonia solution in methanol for the detection of positively ionisable compounds. Under these optimized chromatographic conditions the investigated compounds were determined via a single chromatographic run, with only one polarity switch, in 15min, achieving the following instrumental detection limits: 600pg for AP1EOs, 0.8-14pg for AP2EOs, 10.4-150pg for APs and 4.4-4.8pg for APECs. The chromatographic method was coupled with solid-phase extraction and clean-up procedures and successfully applied to the analysis of wastewater and surface water samples, highlighting mean concentration ranging from 6ng/L for 4-t-OP1EC to 1434ng/L for 4-NP1121EC, depending on the sample analysed. Copyright © 2014 Elsevier B.V. All rights reserved.

In situ ionic liquid dispersive liquid-liquid microextraction and direct microvial insert thermal desorption for gas chromatographic determination of bisphenol compounds.

PubMed

Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

2016-01-01

A new procedure based on direct insert microvial thermal desorption injection allows the direct analysis of ionic liquid extracts by gas chromatography and mass spectrometry (GC-MS). For this purpose, an in situ ionic liquid dispersive liquid-liquid microextraction (in situ IL DLLME) has been developed for the quantification of bisphenol A (BPA), bisphenol Z (BPZ) and bisphenol F (BPF). Different parameters affecting the extraction efficiency of the microextraction technique and the thermal desorption step were studied. The optimized procedure, determining the analytes as acetyl derivatives, provided detection limits of 26, 18 and 19 ng L(-1) for BPA, BPZ and BPF, respectively. The release of the three analytes from plastic containers was monitored using this newly developed analytical method. Analysis of the migration test solutions for 15 different plastic containers in daily use identified the presence of the analytes at concentrations ranging between 0.07 and 37 μg L(-1) in six of the samples studied, BPA being the most commonly found and at higher concentrations than the other analytes.

A sensitive high-performance liquid chromatographic method for the determination of 6-mercaptopurine in plasma using precolumn derivatization and fluorescence detection.

PubMed

Warren, D J; Slørdal, L

1993-02-01

A sensitive high-performance liquid chromatographic (HPLC) method for measuring plasma concentrations of 6-mercaptopurine (6-MP) is described. After protein precipitation with 5-sulfosalicylic acid, samples are subjected to precolumn derivatization using the thiol-reactive fluorophore monobromobimane (mBrB). The drug-mBrB adduct is then resolved by isocratic elution from a C18 reversed-phase support and quantified by fluorescence detection. Recovery of 6-MP after protein precipitation was consistently > 85% and the drug-mBrB adduct was found to be stable for at least 2 weeks at room temperature. With plasma samples containing 30 nM 6-MP, the assay displayed within-run (n = 6) and between-day (n = 6) coefficients of variation of 2.2 and 10.6%, respectively. The limit of detection for 6-MP in plasma was 3 nM (500 pg/ml) and the standard curve was linear up to 3 microM. Using this method, we have observed that 6-MP is stable in heparinized whole blood for at least 24 h provided samples are maintained on ice. Since this method requires few manipulations during sample preparation and is readily adaptable to automated techniques, it may prove useful in the routine clinical laboratory setting.

Improving LC-MS sensitivity through increases in chromatographic performance: comparisons of UPLC-ES/MS/MS to HPLC-ES/MS/MS.

PubMed

Churchwell, Mona I; Twaddle, Nathan C; Meeker, Larry R; Doerge, Daniel R

2005-10-25

Recent technological advances have made available reverse phase chromatographic media with a 1.7 microm particle size along with a liquid handling system that can operate such columns at much higher pressures. This technology, termed ultra performance liquid chromatography (UPLC), offers significant theoretical advantages in resolution, speed, and sensitivity for analytical determinations, particularly when coupled with mass spectrometers capable of high-speed acquisitions. This paper explores the differences in LC-MS performance by conducting a side-by-side comparison of UPLC for several methods previously optimized for HPLC-based separation and quantification of multiple analytes with maximum throughput. In general, UPLC produced significant improvements in method sensitivity, speed, and resolution. Sensitivity increases with UPLC, which were found to be analyte-dependent, were as large as 10-fold and improvements in method speed were as large as 5-fold under conditions of comparable peak separations. Improvements in chromatographic resolution with UPLC were apparent from generally narrower peak widths and from a separation of diastereomers not possible using HPLC. Overall, the improvements in LC-MS method sensitivity, speed, and resolution provided by UPLC show that further advances can be made in analytical methodology to add significant value to hypothesis-driven research.

High-performance liquid chromatographic assay for the determination of novel triazole antifungal agents in tissue. Application to tissue distribution studies.

PubMed

Khan, J K; Montaseri, H; Poglod, M; Bu, H Z; Daneshtalab, M; Micetich, R G

2000-08-01

A simple and rugged reversed-phase high-performance liquid chromatographic method with ultraviolet absorbance detection at 263 nm was developed and validated for the analysis of novel triazole antifungal agents SYN-2869 and its derivatives in tissues. The method involved homogenization with 0.01 M phosphate buffer (pH 7.8) for lung, brain and spleen tissues. The liver and kidneys were homogenized with acetonitrile:acetone (1:1). The plasma proteins were precipitated with ice-cold acetonitrile and supernatent was evaporated to dryness. The reconstituted samples were injected onto an HPLC system. SYN-2869 was separated from the matrix components on a symmetry C(18) column using a aqueous mobile phase of acetonitrile and water with a flow rate of 1 mL/min. A step gradient of 40-80% acetonitrile eluted SYN-2869 and the internal standard (SYN-2506). The linear range was 0.5-10 microgram/g (r(2) > 0.99). The limit of quantitation was 0.5 microgram/g. The inter-day precision and accuracy for SYN 2869 standard concentration were from 2.6 to 7.4% and from -1.56 to +3.29%, respectively. The method was applied to tissue samples collected from single intravenous administration to mice to evaluate the distribution of these novel antifungal agents to different tissues. Copyright 2000 John Wiley & Sons, Ltd.

High-performance liquid chromatographic method for the determination of moclobemide and its two major metabolites in human plasma.

PubMed

Rakic, Anita; Miljkovic, Branislava; Pokrajac, Milena; Vucicevic, Katarina

2007-03-12

A selective, sensitive, and simple high-performance liquid chromatographic (HPLC) method was developed for the determination of moclobemide and its two major metabolites, Ro 12-5637 and Ro 12-8095, in human plasma. Sample preparation (0.5 ml of plasma) involved solid-phase extraction (SPE) using Speedisk H(2)O-Philic DVB columns. Separations were performed on a Waters XTerra RP18 column (5 microm, 150 mm x 4.6 mm). The mobile phase consisted of 10 mM KH(2)PO(4) with 1% triethylamine (pH 3.9) and acetonitrile (83:17, v/v), and a flow-rate was 1.2 ml/min. The total run time was 13 min. UV detection was performed at 240 nm. Mean absolute recoveries were > or =90% and the limit of quantification (LOQ) for all analytes was 0.02 mg/l. Calibration curves were linear (r>0.995) over a wide range of the analyte concentrations in plasma; thus, the method is suitable for different clinical studies when large variations in the drug/metabolites concentrations are observed. During a 5-day assay validation procedure the accuracy and precision were tested and proven (relative errors (RE)< or =13%; intra-day coefficient of variation (CV)< or =7%; inter-day CV< or =13%). Many drugs frequently used in the target patient population were evaluated for potential interference in order method selectivity to be ensured. The assay has been used in a clinical pharmacokinetic study to assess steady-state pharmacokinetics of moclobemide and two metabolites in depressive patients on mono- and combined therapy.

Method to fabricate silicon chromatographic column comprising fluid ports

DOEpatents

Manginell, Ronald P.; Frye-Mason, Gregory C.; Heller, Edwin J.; Adkins, Douglas R.

2004-03-02

A new method for fabricating a silicon chromatographic column comprising through-substrate fluid ports has been developed. This new method enables the fabrication of multi-layer interconnected stacks of silicon chromatographic columns.

Chiral Luttinger liquids and a generalized Luttinger theorem in fractional quantum Hall edges via finite-entanglement scaling

NASA Astrophysics Data System (ADS)

Varjas, Dániel; Zaletel, Michael P.; Moore, Joel E.

2013-10-01

We use bosonic field theories and the infinite system density matrix renormalization group method to study infinite strips of fractional quantum Hall states starting from microscopic Hamiltonians. Finite-entanglement scaling allows us to accurately measure chiral central charge, edge-mode exponents, and momenta without finite-size errors. We analyze states in the first and second levels of the standard hierarchy and compare our results to predictions of the chiral Luttinger liquid theory. The results confirm the universality of scaling exponents in chiral edges and demonstrate that renormalization is subject to universal relations in the nonchiral case. We prove a generalized Luttinger theorem involving all singularities in the momentum-resolved density, which naturally arises when mapping Landau levels on a cylinder to a fermion chain and deepens our understanding of non-Fermi liquids in one dimension.

Fractionation and identification of the allergic proteins in Aspergillus species.

PubMed

Falahati, M; Ghanbari, S; Ebrahimi, M; Ghazanfari, M; Bazrafshan, F; Farahyar, S; Falak, R

2016-12-01

Allergy is an undesired immune response to non-pathogenic agents. However, some opportunistic microorganisms such as fungi can also cause allergy. Among those fungi, hyphae form of Aspergillus strains including A. fumigatus , A. flavus , and A. niger could be mentioned. In this study, we aimed to separate allergic proteins from Aspergillus strains and determine their identity. Standard species of Aspergillus strains were cultivated in optimized conditions and the mycelium was separated by centrifugation. The fungal cells were lysed through physical methods such as freeze-thawing and grinding to prepare a suitable protein extract. The protein concentration was measured by Bradford method and the electrophoretic pattern of the extract was determined by sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). The proteins were fractionated by ammonium sulfate precipitation and anion exchange chromatography using fast protein liquid chromatography (FPLC) system. The IgE immunoreactivity of the sensitized patients and controls was studied using the fractionated proteins by enzyme-linked immunosorbent assay (ELISA). Following SDS-PAGE, proteins were electrotransferred onto polyvinylidene difluoride (PVDF) membranes and the strips were blotted with allergic patients' and controls' sera. The immunoreactive bands were excised from colloidal coomassie-stained SDS-PAGE gels and studied by mass spectroscopy methods. Among the studied species, A. fumigatus showed stronger IgE reactivity and more IgE reactive protein bands than others did. The proteins with higher molecular weights showed stronger immunoreactivity in Western blotting. Receiver operating characteristic curve analysis demonstrated a correlation between the results of the applied ELISA methods. One of the most prominent IgE-reactive proteins was confirmed to be 45 kDa mycelia catalase. Our findings confirmed that high molecular weight proteins might play a major role in allergy and IgE reactivity to

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

PubMed

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

2015-03-01

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

Beyond the Fermi liquid paradigm: Hidden Fermi liquids

PubMed Central

Jain, J. K.; Anderson, P. W.

2009-01-01

An intense investigation of possible non-Fermi liquid states of matter has been inspired by two of the most intriguing phenomena discovered in the past quarter century, namely, high-temperature superconductivity and the fractional quantum Hall effect. Despite enormous conceptual strides, these two fields have developed largely along separate paths. Two widely employed theories are the resonating valence bond theory for high-temperature superconductivity and the composite fermion theory for the fractional quantum Hall effect. The goal of this perspective article is to note that they subscribe to a common underlying paradigm: They both connect these exotic quantum liquids to certain ordinary Fermi liquids residing in unphysical Hilbert spaces. Such a relation yields numerous nontrivial experimental consequences, exposing these theories to rigorous and definitive tests. PMID:19506260

Dissolution and fractionation of nut shells in ionic liquids.

PubMed

Carneiro, Aristides P; Rodríguez, Oscar; Macedo, Eugénia A

2017-03-01

The aim of this work was to study the dissolution of raw peanut and chestnut shells in ionic liquids. Dissolution of raw biomass up to 7wt% was achieved under optimized operatory conditions. Quantification of polysaccharides dissolved through quantitative 13 Cq NMR revealed extractions of the cellulosic material to ionic liquids as high as 87%. Regeneration experiments using an antisolvent mixture allowed to recover the cellulosic material and the ionic liquid. The overall mass balance presented very low loss rates (<8%), recoveries of 75% and 95% of cellulosic material from peanut and chestnut shells, respectively, and the recovery of more than 95% of the ionic liquid in both cases. These results show the high potential of using nut shells and ionic liquids for biorefining purposes. Moreover, high recovery of ionic liquids favors the process from an economical point of view. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of metal ions in tea samples using task-specific ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction coupled to liquid chromatography with ultraviolet detection.

PubMed

Werner, Justyna

2016-04-01

Task-specific ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction was used for the preconcentration of cadmium(II), cobalt(II), and lead(II) ions in tea samples, which were subsequently analyzed by liquid chromatography with UV detection. The proposed method of preconcentration is free of volatile organic compounds, which are often used as extractants and dispersing solvents in classic techniques of microextraction. A task-specific ionic liquid trioctylmethylammonium thiosalicylate was used as an extractant and a chelating agent. Ultrasound was used to disperse the ionic liquid. After microextraction, the phases were separated by centrifugation, and the ionic liquid phase was solubilized in methanol and directly injected into the liquid chromatograph. Selected microextraction parameters, such as the volume of ionic liquid, the pH of the sample, the duration of ultrasound treatment, the speed and time of centrifugation, and the effect of ionic strength, were optimized. Under optimal conditions an enrichment factor of 200 was obtained for each analyte. The limits of detection were 0.002 mg/kg for Cd(II), 0.009 mg/kg for Co(II), and 0.013 mg/kg for Pb(II). The accuracy of the proposed method was evaluated by an analysis of the Certified Reference Materials (INCT-TL-1, INCT-MPH-2) with the recovery values in the range of 90-104%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

Karaźniewicz-Łada, Marta; Główka, Anna

2016-01-01

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

High-performance liquid chromatographic method for the determination and pharmacokinetic study of oxypeucedanin hydrate and byak-angelicin after oral administration of Angelica dahurica extracts in mongrel dog plasma.

PubMed

Xie, Ying; Chen, Yi; Lin, Mei; Wen, Jun; Fan, Guorong; Wu, Yutian

2007-05-09

A high-performance liquid chromatographic method was developed and validated for the determination and pharmacokinetic study of oxypeucedanin hydrate and byak-angelicin after oral administration of Angelica dahurica extracts in mongrel dog plasma. The coumarin components and the internal standard isopsoralen were extracted from plasma samples with the mixture of tert-butyl methyl ether and n-hexane (4:1, v/v). Chromatographic separation was performed on a C(18) column (200 mm x 4.6mm, 5 microm) with the mobile phase acetonitrile-methanol-water-acetic acid (20:15:65:2, v/v/v/v) at a flow-rate of 1.0 ml/min. Only the peak of oxypeucedanin hydrate and byak-angelicin could be detected in dog plasma after oral administration of ethanol extracts of A. dahurica mainly containing xanthotoxol, osthenol, imperatorin, oxypeucedanin hydrate and byak-angelicin. The calibration curves of oxypeucedanin hydrate and byak-angelicin were linear over a range of 22.08-8830.00 and 6.08-2430.00 ng/ml in dog plasma, respectively. The quantification limit of oxypeucedanin hydrate and byak-angelicin in dog plasma was 22.08 and 6.08 ng/ml, respectively. The intra- and inter-day precision was less than 7.6% and 8.5% and the accuracy was from 91.9% to 106.1%. The lowest absolute recoveries of oxypeucedanin hydrate and byak-angelicin were 85.7% and 87.0%, respectively. The method was successfully applied to the pharmacokinetic studies of oxypeucedanin hydrate and byak-angelicin in dog plasma after oral administration of ethanol extracts from A. dahurica.

Investigation of structural changes of β-casein and lysozyme at the gas-liquid interface during foam fractionation.

PubMed

Barackov, Ivana; Mause, Anika; Kapoor, Shobhna; Winter, Roland; Schembecker, Gerhard; Burghoff, Bernhard

2012-10-15

Purification and separation of proteins play a major role in biotechnology. Nowadays, alternatives to multistep operations suffering from low product yields and high costs are investigated closely amidst which one of the promising options is foam fractionation. The molecular behavior at the gas-liquid interface plays an important role in the formation and stabilization of enriched foam. This study for the first time correlates the physico-chemical parameters to the molecular structure in view of protein enrichment during foam fractionation of the two relatively different proteins lysozyme and β-casein employing biophysical techniques such as circular dichroism (CD) spectroscopy and infrared reflection absorption spectroscopy (IRRAS). In case of lysozyme, high enrichment was achieved at pHliquid interface, depending on favorable or unfavorable conditions. Copyright © 2012 Elsevier B.V. All rights reserved.

SEPARATION AND CHARACTERIZATION OF TETROL METABOLITES OF BENZO[A]PYRENE-DNA ADDUCTS USING HPLC AND SOLID-MATRIX ROOM TEMPERATURE LUMINESCENCE. (R824100)

EPA Science Inventory

Abstract

Four tetrols of benzo[a]pyrene-DNA adducts were separated using reversed-phase high performance liquid chromatography. Chromatographic fractions containing a given tetrol were readily characterized with solid-matrix room temperature luminescence techniques. So...

CHROMATOGRAPHIC TECHNIQUES IN PHARMACEUTICAL ANALYSIS IN POIAND: HISTORY AND THE PRESENCE ON THE BASIS OF PAPERS PUBLISHED IN SELECTED POLISH PHARMACEUTICAL JOURNALS IN XX CENTURY.

PubMed

Bilek, Maciej; Namieśnik, Jacek

2016-01-01

For a long time, chromatographic techniques and techniques related to them have stimulated the development of new procedures in the field of pharmaceutical analysis. The newly developed methods, characterized by improved metrological parameters, allow for more accurate testing of, among others, the composition of raw materials, intermediates and final products. The chromatographic techniques also enable studies on waste generated in research laboratories and factories producing pharmaceuticals and parapharmaceuticals. Based on the review of reports published in Polish pharmaceutical journals, we assessed the impact of chromatographic techniques on the development of pharmaceutical analysis. The first chromatographic technique used in pharmaceutical analysis was a so-called capillary analysis. It was applied in the 1930s to control the identity of pharmaceutical formulations. In the 1940s and 1950s, the chromatographic techniques were mostly a subject of review publications, while their use in experimental work was rare. Paper chromatography and thin layer chromatography were introduced in the 1960s and 1970s, respectively. These new analytical tools have contributed to the intensive development of research in the field of phytochemistry and the analysis of herbal medicines. The development of colunm chromatography-based techniques, i.e., gas chromatography and high performance liquid chromatography took place in the end of 20th century. Both aforementioned techniques were widely applied in pharmaceutical analysis, for example, to assess the stability of drugs, test for impurities and degradation products as well as in pharmacokinetics studies. The first decade of 21" century was the time of new detection methods in gas and liquid chromatography. The information sources used to write this article were Polish pharmaceutical journals, both professional and scientific, originating from the interwar and post-war period, i.e., "Kronika Farmaceutyczna", "Farmacja Wsp

Analysis of essential oils and fragrances with a new generation of highly inert gas chromatographic columns coated with ionic liquids.

PubMed

Cagliero, Cecilia; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

2017-04-28

In the fields of essential oils and fragrances, samples often consist of mixtures of compounds with similar structural and physical characteristics (e.g. mono- and sesquiterpenoids), whose correct identification closely depends on the synergic combination of chromatographic and mass spectral data. This sample complexity means that new GC stationary phases with different selectivities are continually being investigated. Ionic liquids (ILs) are of great interest as GC stationary phases in this field because of their selectivity (significantly different than that of currently phases) and their high temperature stability. A first generation of IL GC columns was found to be competitive when applied to these field, in terms of selectivity and efficiency, compared to conventional columns (polydimethylsiloxane, (e.g. OV-1), methyl-polysiloxane 5%-phenyl (e.g. SE-52), 7%-cyanopropyl, 7%-phenyl polysiloxane (e.g. OV-1701), and polyethylen glycol (e.g. PEG-20M). However, these columns showed significant activity towards polar or active analytes, which primarily affected their quantitative performance. A new generation of highly-inactive columns coated with three of the most widely-used ionic liquid GC stationary phases has recently been introduced; these phases are SLB-IL60i (1,12-di(tripropylphosphonium) dodecane bis(trifluoromethylsulfonyl) imide [NTf 2 ], SLB-IL76i (tri-(tripropylphosphonium-hexanamido)-triethylamine [NTf 2 ]), and SLB-IL111i (1,5-di (2,3-dimethyllimidazolium) pentane [NTf 2 ]). This study carefully tested the new inert IL columns, in view of their routine application in the fragrance and essential oil fields. They were found to have unusually high selectivity, comparable to that of first-generation IL columns, while their inertness and efficiency were competitive with those of currently-used conventional columns. The IL column performance of first and second generations was compared, through the quali-quantitative analysis of components in a group of

Ultra-sensitive assay for paclitaxel in intracellular compartments of A549 cells using liquid chromatography-tandem mass spectrometry.

PubMed

Wang, Tingting; Ma, Wenxiao; Sun, Yantong; Yang, Yan; Zhang, Weiping; Fawcett, J Paul; Du, Hongwei; Gu, Jingkai

2013-01-01

A high-performance liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the determination of paclitaxel in intracellular compartments using docetaxel as internal standard (IS) has been developed and validated. A549 cancer cells (10(6)) were incubated with paclitaxel (2ng/mL) for up to 4h and then subjected to sequential extraction of cytosolic, membrane/organelle, nuclear and cytoskeleton soluble protein. Fractions were ultrasonicated to release protein bound paclitaxel after which drug was extracted using liquid-liquid extraction with diethyl ether:dichloromethane (2:1, v/v). Chromatographic separation was then carried out on an Ascentis Express C18 column (50mm×4.6mm, 2.7μm) with a mobile phase of acetonitrile:0.1% formic acid in water (50:50, v/v). Detection involved electrospray positive ionization followed by multiple reactions monitoring of the precursor-to-product ion transitions of paclitaxel at m/z 854.4→286.3 and docetaxel at m/z 808.6→226.1. Assay validation based on samples of total cell extract in the same buffer as protein fractions showed the assay was linear over the range 2-600pg/mL with intra- and inter-day precision (as relative standard deviation) and accuracy (as relative error) of <7% and <±12%, respectively. Recovery was approximately 70% and matrix effects were minimal. The distribution of paclitaxel in subcellular components of A549 cancer cells was mainly into the cytoskeletal compartment. Copyright © 2012 Elsevier B.V. All rights reserved.

Crude extract and fractions from Eugenia uniflora Linn leaves showed anti-inflammatory, antioxidant, and antibacterial activities.

PubMed

Falcão, Tamires Rocha; de Araújo, Aurigena Antunes; Soares, Luiz Alberto Lira; de Moraes Ramos, Rhayanne Thaís; Bezerra, Isabelle Cristinne Ferraz; Ferreira, Magda Rhayanny Assunção; de Souza Neto, Manoel André; Melo, Maria Celeste Nunes; de Araújo, Raimundo Fernandes; de Aguiar Guerra, Andreza Conceição Véras; de Medeiros, Juliana Silva; Guerra, Gerlane Coelho Bernardo

2018-03-09

This study showed phytochemical composition and evaluates the anti-inflammatory, and analgesic activities of crude extract (CE) and fractions from E. uniflora Linn leaves. Polyphenols present in crude extract (CE), in aqueous fraction (AqF), and ethyl acetate (EAF) treated fractions from E. uniflora Linn leaves were shown by chromatographic analysis in order to conduct a phytochemical characterization. Antibacterial activity was evaluated based on minimum inhibitory concentrations (MICs) determined using the agar dilution method. Doses of 50, 100, and 200 mg/kg of the CE and fractions were applied for conducting in vivo models (male Swiss mice, 8-10 weeks old). The peritonitis experimental model was induced by carrageenan following of Myeloperoxidase activity (MPO), Total glutathione and malondialdehyde (MDA), IL-1β and TNF-α levels by spectroscopic UV/VIS analysis. Antinociceptive activity was evaluated based on an abdominal writhing model and hot plate test. The results were statistically evaluated using one-way analysis of variance (ANOVA), followed by Bonferroni's post-hoc test. The level of statistical significance was p < 0.05. High-performance liquid chromatography with photodiode array detection (HPLC-DAD) detected varying concentrations of gallic acid, ellagic acid, and myricitrin in the CE and fractions obtained from E. uniflora Linn leaves (0.05-0.87%w/w, 0.20-0.32%w/w, and 1.71-6.56%w/w, respectively). In general, the CE had lower MIC values than the fractions, including the lowest MIC against the MRSA strain. The CE and AqF also significantly reduced leukocyte migration and MPO activity (p < 0.05). In addition, AqF significantly reduced IL-1β and TNF-α levels (p < 0.05). Furthermore, the CE and fractions exhibited an antioxidant effect (p < 0.05) and peripheral analgesic activity (p < 0.05). The CE and fractions from the studied E. uniflora Linn leaves exhibited antibacterial, anti-inflammatory, antioxidant, and analgesic

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

PubMed

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

2013-01-01

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

Simple gas chromatographic method for furfural analysis.

PubMed

Gaspar, Elvira M S M; Lopes, João F

2009-04-03

A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSD<8%), showed good recoveries (77-107%) and good limits of detection (GC-FID: 1.37 microgL(-1) for 2-F, 8.96 microgL(-1) for 5-MF, 6.52 microgL(-1) for 5-HMF; GC-TOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet.

Chromatographic Studies of Protein-Based Chiral Separations

PubMed Central

Bi, Cong; Zheng, Xiwei; Azaria, Shiden; Beeram, Sandya; Li, Zhao; Hage, David S.

2016-01-01

The development of separation methods for the analysis and resolution of chiral drugs and solutes has been an area of ongoing interest in pharmaceutical research. The use of proteins as chiral binding agents in high-performance liquid chromatography (HPLC) has been an approach that has received particular attention in such work. This report provides an overview of proteins that have been used as binding agents to create chiral stationary phases (CSPs) and in the use of chromatographic methods to study these materials and protein-based chiral separations. The supports and methods that have been employed to prepare protein-based CSPs will also be discussed and compared. Specific types of CSPs that are considered include those that employ serum transport proteins (e.g., human serum albumin, bovine serum albumin, and alpha1-acid glycoprotein), enzymes (e.g., penicillin G acylase, cellobiohydrolases, and α-chymotrypsin) or other types of proteins (e.g., ovomucoid, antibodies, and avidin or streptavidin). The properties and applications for each type of protein and CSP will also be discussed in terms of their use in chromatography and chiral separations. PMID:28344977

Pharmacognostic Screening of Piper trichostachyon Fruits and its Comparative Analysis with Piper nigrum Using Chromatographic Techniques.

PubMed

Upadhya, Vinayak; Pai, Sandeep R; Ankad, Gireesh M; Hegde, Harsha V

2016-05-01

Piper trichostachyon is a wild, endemic Piper species from Western Ghats of India. The folklore healers of Belagavi region use this plant, similar to Piper nigrum. The present study investigates the comparison between P. nigrum and P. trichostachyon using pharmacognostic parameters. Pharmacognostic evaluation was carried out in terms of morphological, microscopic characters, and phytochemical analysis using standard methods. Comparative physicochemical analysis between P. trichostachyon and P. nigrum was also carried out through estimation of micro-macro nutrients, high-performance thin layer chromatography (HPTLC) investigation and using piperine as a marker compound for reversed phase-ultra flow liquid chromatographic (RP-UFLC) technique. P. trichostachyon grows in the forests, and the fruits are morphologically similar to P. nigrum fruits, so the name in Kannada "Kaadu Kalu menasu" (wild/forest black pepper). The microscopy revealed the presence of stone cells, starch grains, oil cells and globules, beaker cells, and yellowish brown pigment layer, parenchymatous cells. The presence of alkaloids, oil, and tannins were observed in P. trichostachyon fruits. The HPTLC studies visibly indicated differences among two species with 12 peaks and varied banding pattern. RP-UFLC results showed less amount of piperine in P. trichostachyon (0.05 ± 0.002 mg/g) than in P. nigrum (16.14 ± 0.807 mg/g). The study reports on pharmacognostic parameters of P. trichostachyon for the 1(st) time and will be useful for the identification and authentication. The comparative HPTLC and RP-UFLC studies resolve the differentiation impasse among two species. However, further biological efficacy studies are required to establish its use in traditional medicine. Piper trichostachyon grows in the forests, and the fruits are morphologically similar to Piper nigrum fruitsThe microscopy of P. trichostachyon revealed the presence of stone cells, starch grains, oil cells and globules, beaker cells

Pharmacognostic Screening of Piper trichostachyon Fruits and its Comparative Analysis with Piper nigrum Using Chromatographic Techniques

PubMed Central

Upadhya, Vinayak; Pai, Sandeep R.; Ankad, Gireesh M.; Hegde, Harsha V.

2016-01-01

Background: Piper trichostachyon is a wild, endemic Piper species from Western Ghats of India. The folklore healers of Belagavi region use this plant, similar to Piper nigrum. Aims: The present study investigates the comparison between P. nigrum and P. trichostachyon using pharmacognostic parameters. Materials and Methods: Pharmacognostic evaluation was carried out in terms of morphological, microscopic characters, and phytochemical analysis using standard methods. Comparative physicochemical analysis between P. trichostachyon and P. nigrum was also carried out through estimation of micro-macro nutrients, high-performance thin layer chromatography (HPTLC) investigation and using piperine as a marker compound for reversed phase-ultra flow liquid chromatographic (RP-UFLC) technique. Results: P. trichostachyon grows in the forests, and the fruits are morphologically similar to P. nigrum fruits, so the name in Kannada “Kaadu Kalu menasu” (wild/forest black pepper). The microscopy revealed the presence of stone cells, starch grains, oil cells and globules, beaker cells, and yellowish brown pigment layer, parenchymatous cells. The presence of alkaloids, oil, and tannins were observed in P. trichostachyon fruits. The HPTLC studies visibly indicated differences among two species with 12 peaks and varied banding pattern. RP-UFLC results showed less amount of piperine in P. trichostachyon (0.05 ± 0.002 mg/g) than in P. nigrum (16.14 ± 0.807 mg/g). Conclusion: The study reports on pharmacognostic parameters of P. trichostachyon for the 1st time and will be useful for the identification and authentication. The comparative HPTLC and RP-UFLC studies resolve the differentiation impasse among two species. However, further biological efficacy studies are required to establish its use in traditional medicine. SUMMARY Piper trichostachyon grows in the forests, and the fruits are morphologically similar to Piper nigrum fruitsThe microscopy of P. trichostachyon revealed the

Chiral Luttinger liquids and a generalized Luttinger's theorem in fractional quantum Hall edges via finite-entanglement scaling

NASA Astrophysics Data System (ADS)

Varjas, Daniel; Zaletel, Michael; Moore, Joel

2014-03-01

We use bosonic field theories and the infinite system density matrix renormalization group (iDMRG) method to study infinite strips of fractional quantum Hall (FQH) states starting from microscopic Hamiltonians. Finite-entanglement scaling allows us to accurately measure chiral central charge, edge mode exponents and momenta without finite-size errors. We analyze states in the first and second level of the standard hierarchy and compare our results to predictions of the chiral Luttinger liquid (χLL) theory. The results confirm the universality of scaling exponents in chiral edges and demonstrate that renormalization is subject to universal relations in the non-chiral case. We prove a generalized Luttinger's theorem involving all singularities in the momentum-resolved density, which naturally arises when mapping Landau levels on a cylinder to a fermion chain and deepens our understanding of non-Fermi liquids in 1D.

A high-resolution peak fractionation approach for streamlined screening of nuclear-factor-E2-related factor-2 activators in Salvia miltiorrhiza.

PubMed

Zhang, Hui; Luo, Li-Ping; Song, Hui-Peng; Hao, Hai-Ping; Zhou, Ping; Qi, Lian-Wen; Li, Ping; Chen, Jun

2014-01-24

Generation of a high-purity fraction library for efficiently screening active compounds from natural products is challenging because of their chemical diversity and complex matrices. In this work, a strategy combining high-resolution peak fractionation (HRPF) with a cell-based assay was proposed for target screening of bioactive constituents from natural products. In this approach, peak fractionation was conducted under chromatographic conditions optimized for high-resolution separation of the natural product extract. The HRPF approach was automatically performed according to the predefinition of certain peaks based on their retention times from a reference chromatographic profile. The corresponding HRPF database was collected with a parallel mass spectrometer to ensure purity and characterize the structures of compounds in the various fractions. Using this approach, a set of 75 peak fractions on the microgram scale was generated from 4mg of the extract of Salvia miltiorrhiza. After screening by an ARE-luciferase reporter gene assay, 20 diterpene quinones were selected and identified, and 16 of these compounds were reported to possess novel Nrf2 activation activity. Compared with conventional fixed-time interval fractionation, the HRPF approach could significantly improve the efficiency of bioactive compound discovery and facilitate the uncovering of minor active components. Copyright © 2013 Elsevier B.V. All rights reserved.

Analysis of imazaquin in soybeans by solid-phase extraction and high-performance liquid chromatography.

PubMed

Guo, C; Hu, J-Y; Chen, X-Y; Li, J-Z

2008-02-01

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

Isolation of an Antioxidative Substance Produced by Aspergillus repens.

PubMed

Yagi, R; Doi, M

1999-01-01

The acidic fraction of an extract of the culture liquid of Aspergillus repens MA0197 showed strong antioxidative activity when tested by the ferric thiocyanate and TBA methods. Chromatographic purification of this acidic fraction gave an active substance identified as Neoechinulin A. This compound showed higher antioxidative activity than α-tocopherol and could be expected to act as an antioxidant in Katsuobushi.

Development and Bioanalytical Validation of a Liquid Chromatographic-Tandem Mass Spectrometric (LC-MS/MS) Method for the Quantification of the CCR5 Antagonist Maraviroc in Human Plasma

PubMed Central

Emory, Joshua F.; Seserko, Lauren A.; Marzinke, Mark A.

2014-01-01

Background Maraviroc is a CCR5 antagonist that has been utilized as a viral entry inhibitor in the management of HIV-1. Current clinical trials are pursuing maraviroc drug efficacy in both oral and topical formulations. Therefore, in order to fully understand drug pharmacokinetics, a sensitive method is required to quantify plasma drug concentrations. Methods Maraviroc-spiked plasma was combined with acetonitrile containing an isotopically-labeled internal standard, and following protein precipitation, samples were evaporated to dryness and reconstituted for liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis. Chromatographic separation was achieved on a Waters BEH C8, 50 × 2.1 mm UPLC column, with a 1.7 μm particle size and the eluent was analyzed using an API 4000 mass analyzer in selected reaction monitoring mode. The method was validated as per FDA Bioanalytical Method Validation guidelines. Results The analytical measuring range of the LC-MS/MS method is 0.5-1000 ng/ml. Calibration curves were generated using weighted 1/x2 quadratic regression. Inter-and intra-assay precision was ≤ 5.38% and ≤ 5.98%, respectively; inter-and intra-assay accuracy (%DEV) was ≤ 10.2% and ≤ 8.44%, respectively. Additional studies illustrated similar matrix effects between maraviroc and its internal standard, and that maraviroc is stable under a variety of conditions. Method comparison studies with a reference LC-MS/MS method show a slope of 0.948 with a Spearman coefficient of 0.98. Conclusions Based on the validation metrics, we have generated a sensitive and automated LC-MS/MS method for maraviroc quantification in human plasma. PMID:24561264

Methods to control phase inversions and enhance mass transfer in liquid-liquid dispersions

DOEpatents

Tsouris, Constantinos; Dong, Junhang

2002-01-01

The present invention is directed to the effects of applied electric fields on liquid-liquid dispersions. In general, the present invention is directed to the control of phase inversions in liquid-liquid dispersions. Because of polarization and deformation effects, coalescence of aqueous drops is facilitated by the application of electric fields. As a result, with an increase in the applied voltage, the ambivalence region is narrowed and shifted toward higher volume fractions of the dispersed phase. This permits the invention to be used to ensure that the aqueous phase remains continuous, even at a high volume fraction of the organic phase. Additionally, the volume fraction of the organic phase may be increased without causing phase inversion, and may be used to correct a phase inversion which has already occurred. Finally, the invention may be used to enhance mass transfer rates from one phase to another through the use of phase inversions.

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

NASA Astrophysics Data System (ADS)

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

2014-02-01

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

Supramolecular solvent-based extraction of benzimidazolic fungicides from natural waters prior to their liquid chromatographic/fluorimetric determination.

PubMed

Moral, Antonia; Sicilia, María Dolores; Rubio, Soledad

2009-05-01

A supramolecular solvent made up of vesicles of decanoic acid in the nano- and microscale regimes dispersed in a continuous aqueous phase is proposed for the extraction/preconcentration of benzimidazolic fungicides (BFs) from river and underground water samples prior to their determination by liquid chromatography (LC)/fluorimetry. The solvent is produced from the coacervation of decanoic acid aqueous vesicles by the action of tetrabutylammonium (Bu(4)N(+)). Carbendazim (CB), thiabendazole (TB) and fuberidazole (FB) are extracted on the basis of hydrophobic and pi-cation interactions and the formation of hydrogen bonds. The extraction provides high preconcentration factors (160 for CB and 190 for TB and FB), requires a short time (the procedure takes less than 20 min and several samples can be simultaneously processed) and a low sample volume (20 mL), and avoids the use of toxic organic solvents. Because of the absence of matrix interferences and the low viscosity of the extracts, these can be directly injected into the chromatographic system without the need of cleaning-up or diluting them. Recoveries are not influenced by the presence of salt concentrations up to 1 M. The proposed method provides detection limits for the determination of CB, TB and FB in natural waters of 32, 4 and 0.1 ng L(-1), respectively, and a precision, expressed as relative standard deviation (n=11) of 5.5% for CB (100 ng L(-1)), 4.0% for TB (80 ng L(-1)) and 2.5% for FB (30 ng L(-1)). Recoveries obtained by applying this approach to the analysis of river and underground water samples fortified at the ng L(-1) level are in the intervals 75-83, 95-102 and 97-101% for CB, TB and FB, respectively.

Reductive amination of glutaraldehyde 2,4-dinitrophenylhydrazone using 2-picoline borane and high-performance liquid chromatographic analysis.

PubMed

Uchiyama, Shigehisa; Sakamoto, Hironari; Ohno, Akiko; Inaba, Yohei; Nakagome, Hideki; Kunugita, Naoki

2012-09-21

A typical method for the measurement of glutaraldehyde (GLA) employs 2,4-dinitrophenylhydrazine (DNPH) to form GLA-DNPhydrazone derivatives. However, this method is subject to analytical errors because GLA-DNPhydrazone is a quaternary bis-derivative and forms three geometric isomers (E-E, E-Z and Z-Z) as a result of the two C[double bond, length as m-dash]N double bonds. To overcome this issue, a method for transforming the C[double bond, length as m-dash]N double bond into a C-N single bond, using reductive amination of DNPhydrazone derivatives, has been applied. The amination reaction of GLA-DNPhydrazones with 2-picoline borane is accelerated with catalytic amounts of acid and is completed within 10 minutes in the presence of 100 mmol L(-1) phosphoric acid. Reduction of GLA-DNPhydrazone by 2-picoline borane is unique and results in the formation of N-(2,4-dinitrophenyl)-1-piperidinamine (DNPPA). NMR and LC-APCI-MS data confirmed the product identification. DNPPA is very stable and did not change when stored for at least four weeks at room temperature. DNPPA has excellent solubility of 14.6 g L(-1) at 20 °C in acetonitrile. The absorption maximum wavelength and the molar absorptivity of DNPPA were 351 nm and 4.2 × 10(4) L mol(-1) cm(-1) respectively. Complete separation between the reduced forms of C1-C10 aldehyde DNPhydrazones, including DNPPA, can be achieved by operating the reversed-phase high-performance liquid chromatograph at 351 nm in gradient mode using a C18 amide column. The reductive amination method for GLA overcomes analytical errors caused by E-E, E-Z and Z-Z geometrical isomers.

Development and validation of a reversed-phase ion-pair high-performance liquid chromatographic method for the determination of risedronate in pharmaceutical preparations.

PubMed

Kyriakides, Demetra; Panderi, Irene

2007-02-12

A stability indicating, reversed-phase ion-pair high-performance liquid chromatographic method was developed and validated for the determination of risedronate in pharmaceutical dosage forms. The determination was performed on a BDS C(18) analytical column (250 mm x 4.6 mm i.d., 5 microm particle size); the mobile phase consisted of 0.005 M tetrabutylammonium hydroxide and 0.005 M pyrophosphate sodium (pH 7.0) mixed with acetonitrile in a ratio (78:22, v/v) and pumped at a flow rate 1.00 mL min(-1). The ultraviolet (UV) detector was operated at 262 nm. The retention times of magnesium ascorbyl phosphate, which was used as internal standard and risedronate were 4.94 and 5.95 min, respectively. The calibration graph was ranged from 2.50 to 20.00 microg mL(-1), while detection and quantitation limits were found to be 0.48 and 1.61 microg mL(-1), respectively. The intra- and inter-day percentage relative standard deviations, %R.S.D., were less than 5.9%, while the relative percentage error, %E(r), was less than 0.4%. The method was applied to the quality control of commercial tablets and content uniformity test and proved to be suitable for rapid and reliable quality control.

Fractional Wigner Crystal in the Helical Luttinger Liquid.

PubMed

Traverso Ziani, N; Crépin, F; Trauzettel, B

2015-11-13

The properties of the strongly interacting edge states of two dimensional topological insulators in the presence of two-particle backscattering are investigated. We find an anomalous behavior of the density-density correlation functions, which show oscillations that are neither of Friedel nor of Wigner type: they, instead, represent a Wigner crystal of fermions of fractional charge e/2, with e the electron charge. By studying the Fermi operator, we demonstrate that the state characterized by such fractional oscillations still bears the signatures of spin-momentum locking. Finally, we compare the spin-spin correlation functions and the density-density correlation functions to argue that the fractional Wigner crystal is characterized by a nontrivial spin texture.

Experimental evidence for the absence of iron isotope fractionation between metal and silicate liquids at 1 GPa and 1250-1300 °C and its cosmochemical consequences

NASA Astrophysics Data System (ADS)

Hin, Remco C.; Schmidt, Max W.; Bourdon, Bernard

2012-09-01

Iron isotope fractionation during metal-silicate differentiation has been proposed as a cause for differences in iron isotope compositions of chondrites, iron meteorites and the bulk silicate Earth. Stable isotope fractionation, however, rapidly decreases with increasing temperature. We have thus performed liquid metal-liquid silicate equilibration experiments at 1250-1300 °C and 1 GPa to address whether Fe isotope fractionation is resolvable at the lowest possible temperatures for magmatic metal-silicate differentiation. A centrifuging piston cylinder apparatus enabled quantitative metal-silicate segregation. Elemental tin or sulphur was used in the synthetic metal-oxide mixtures to lower the melting temperature of the metal. The analyses demonstrate that eight of the 10 experimental systems equilibrated in a closed isotopic system, as was assessed by varying run durations and starting Fe isotope compositions. Statistically significant iron isotope fractionation between quenched metals and silicates was absent in nine of the 10 experiments and all 10 experiments yield an average metal-silicate fractionation factor of 0.01 ± 0.04‰, independent of whether graphite or silica glass capsules were used. This implies that Fe isotopes do not fractionate during low pressure metal-silicate segregation under magmatic conditions. In large bodies such as the Earth, fractionation between metal and high pressure (>20 GPa) silicate phases may still be a possible process for equilibrium fractionation during metal-silicate differentiation. However, the 0.07 ± 0.02‰ heavier composition of bulk magmatic iron meteorites relative to the average of bulk ordinary/carbonaceous chondrites cannot result from equilibrium Fe isotope fractionation during core segregation. The up to 0.5‰ lighter sulphide than metal fraction in iron meteorites and in one ordinary chondrite can only be explained by fractionation during subsolidus processes.

Determination of alternative preservatives in cosmetic products by chromophoric derivatization followed by vortex-assisted liquid-liquid semimicroextraction and liquid chromatography.

PubMed

Miralles, Pablo; Vrouvaki, Ilianna; Chisvert, Alberto; Salvador, Amparo

2016-07-01

An analytical method for the simultaneous determination of phenethyl alcohol, methylpropanediol, phenylpropanol, caprylyl glycol, and ethylhexylglycerin, which are used as alternative preservatives in cosmetic products, has been developed. The method is based on liquid chromatography with UV spectrophotometric detection after chromophoric derivatization with benzoyl chloride and vortex-assisted liquid-liquid semimicroextraction. Different chromatographic parameters, derivatization conditions, and sample preparation variables were studied. Under optimized conditions, the limits of detection values for the analytes ranged from 0.02 to 0.06µgmL(-1). The method was validated with good recovery values (84-118%) and precision values (3.9-9.5%). It was successfully applied to 10 commercially available cosmetic samples. The good analytical features of the proposed method besides of its environmentally-friendly characteristics, make it useful to carry out the quality control of cosmetic products containing the target compounds as preservative agents. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of solvent composition in the normal-phase liquid chromatography of alkylphenols and naphthols

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

Hurtubise, R.J.; Hussain, A.; Silver, H.F.

1981-11-01

The normal-phase liquid chromatographic models of Scott, Snyder, and Soczewinski were considered for a ..mu..-Bondapak NH/sub 2/ stationary phase. n-Heptane:2-propanol and n-heptane:ethyl acetate mobile phases of different compositions were used. Linear relationships were obtained from graphs of log K' vs. log mole fraction of the strong solvent for both n-heptane:2-propanol and n-heptane:ethyl acetate mobile phases. A linear relationship was obtained between the reciprocal of corrected retention volume and % wt/v of 2-propanol but not between the reciprocal of corrected retention volume and % wt/v of ethyl acetate. The slopes and intercept terms from the Snyder and Soczewinski models were foundmore » to approximately describe interactions with ..mu..-Bondapak NH/sub 2/. Capacity factors can be predicted for the compounds by using the equations obtained from mobile phase composition variation experiments.« less

High pressure liquid chromatographic determination of aflatoxins in spices.

PubMed

Awe, M J; Schranz, J L

1981-11-01

High pressure liquid chromatography with fluorescence detection is used to determine aflatoxin in 5 common spices. A 10 micrometer microparticulate silica gel column is used with a dichloromethane-cyclohexane-acetonitrile solvent system to resolve aflatoxins B1, G1, B2, and G2. The fluorescence detector contained a silica gel-packed flowcell. Samples of black, white, and red pepper, ginger, and nutmeg were extracted according to a previously published method. Recoveries from aflatoxin-free samples of white pepper, ginger, and red pepper spiked with 1-50 micrograms aflatoxin/kg ranged from 64 to 92%.

Fractionalization beyond Luttinger Liquid in the spectroscopy of Lithium Purple Bronze

NASA Astrophysics Data System (ADS)

Natalia, Lera; Jose, Alvarez

We offer an interpretation for the departures of ARPES and STS spectroscopies experiments in quasi-one-dimensional Lithium Purple Bronze (LiPB) from single-band Luttinger Liquid (LL) theory. We base our calculation on a phenomenological description of the published data proposed in the original experiments and consider two bands crossing the Fermi level. We discuss the breakdown of the LL scaling relation η = α - 1 , the separation of the spinon edge and the holon peak, the phenomenological TL fit to the Energy Distribution Curves (EDC) and the survival of power-like density of states down to 4K. We consider non-critical fluctuations in one of the separated modes in which the electron fractionalize, and discuss under which conditions could be related with the upturn in the resistivity at 20-30K. We discuss the possibility of a gap in such separated mode and its role on the robust one-dimensional behavior. The connection with the proposed triplet superconductivity is at T = 1 . 4 K is also studied. We acknowledge financial support from MINECO FIS2012-37549-C05-03.

Rapid on-site sensing aflatoxin B1 in food and feed via a chromatographic time-resolved fluoroimmunoassay.

PubMed

Zhang, Zhaowei; Tang, Xiaoqian; Wang, Du; Zhang, Qi; Li, Peiwu; Ding, Xiaoxia

2015-01-01

Aflatoxin B1 poses grave threats to food and feed safety due to its strong carcinogenesis and toxicity, thus requiring ultrasensitive rapid on-site determination. Herein, a portable immunosensor based on chromatographic time-resolved fluoroimmunoassay was developed for sensitive and on-site determination of aflatoxin B1 in food and feed samples. Chromatographic time-resolved fluoroimmunoassay offered a magnified positive signal and low signal-to-noise ratio in time-resolved mode due to the absence of noise interference caused by excitation light sources. Compared with the immunosensing performance in previous studies, this platform demonstrated a wider dynamic range of 0.2-60 μg/kg, lower limit of detection from 0.06 to 0.12 µg/kg, and considerable recovery from 80.5% to 116.7% for different food and feed sample matrices. It was found to be little cross-reactivity with other aflatoxins (B2, G1, G2, and M1). In the case of determination of aflatoxin B1 in peanuts, corn, soy sauce, vegetable oil, and mouse feed, excellent agreement was found when compared with aflatoxin B1 determination via the conversational high-performance liquid chromatography method. The chromatographic time-resolved fluoroimmunoassay affords a powerful alternative for rapid on-site determination of aflatoxin B1 and holds a promise for food safety in consideration of practical food safety and environmental monitoring.

Rapid On-Site Sensing Aflatoxin B1 in Food and Feed via a Chromatographic Time-Resolved Fluoroimmunoassay

PubMed Central

Wang, Du; Zhang, Qi; Li, Peiwu; Ding, Xiaoxia

2015-01-01

Aflatoxin B1 poses grave threats to food and feed safety due to its strong carcinogenesis and toxicity, thus requiring ultrasensitive rapid on-site determination. Herein, a portable immunosensor based on chromatographic time-resolved fluoroimmunoassay was developed for sensitive and on-site determination of aflatoxin B1 in food and feed samples. Chromatographic time-resolved fluoroimmunoassay offered a magnified positive signal and low signal-to-noise ratio in time-resolved mode due to the absence of noise interference caused by excitation light sources. Compared with the immunosensing performance in previous studies, this platform demonstrated a wider dynamic range of 0.2-60 μg/kg, lower limit of detection from 0.06 to 0.12 µg/kg, and considerable recovery from 80.5% to 116.7% for different food and feed sample matrices. It was found to be little cross-reactivity with other aflatoxins (B2, G1, G2, and M1). In the case of determination of aflatoxin B1 in peanuts, corn, soy sauce, vegetable oil, and mouse feed, excellent agreement was found when compared with aflatoxin B1 determination via the conversational high-performance liquid chromatography method. The chromatographic time-resolved fluoroimmunoassay affords a powerful alternative for rapid on-site determination of aflatoxin B1 and holds a promise for food safety in consideration of practical food safety and environmental monitoring. PMID:25874803

Validated high-performance liquid chromatographic method utilizing solid-phase extraction for the simultaneous determination of naringenin and hesperetin in human plasma.

PubMed

Kanaze, Feras Imad; Kokkalou, Eugene; Georgarakis, Manolis; Niopas, Ioannis

2004-03-05

Naringenin and hesperetin, the aglycones of the flavanone glucosides naringin and hesperidin occur naturally in citrus fruits. They exert a variety of pharmacological effects such as antioxidant, blood lipid-lowering, anticarcinogenic and inhibit selected cytochrome P-450 enzymes resulting in drug interactions. A specific, sensitive, precise, and accurate solid-phase extraction high-performance liquid chromatographic (HPLC) assay for the simultaneous determination of naringenin and hesperetin in human plasma was developed and validated. After addition of 7-ethoxycoumarin as internal standard, plasma samples were incubated with beta-glucuronidase/sulphatase, and the analytes were isolated from plasma by solid-phase extraction using C(18) cartridges and separated on a C(8) reversed phase column with methanol/water/acetic acid (40:58:2, v/v/v) as the eluent at 45 degrees C. The method was linear in the 10-300 ng/ml concentration range for both naringenin and hesperetin (r>0.999). Recovery for naringenin, hesperetin and internal standard was greater than 76.7%. Intra- and inter-day precision for naringenin ranged from 1.4 to 4.2% and from 1.9 to 5.2%, respectively, and for hesperetin ranged from 1.3 to 4.1% and from 1.7 to 5.1%, respectively. Accuracy was better than 91.5 and 91.3% for naringenin and hesperetin, respectively.

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

PubMed

Goll, Johannes; Audo, Gregoire; Minceva, Mirjana

2015-08-07

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

Gas-Chromatographic Determination Of Water In Freon PCA

NASA Technical Reports Server (NTRS)

Melton, Donald M.

1994-01-01

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

The Composition of Titan's Lower Atmosphere and Simple Surface Volatiles as Measured by the Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer Experiment

NASA Technical Reports Server (NTRS)

Niemann, H. B.; Atreya, S. K.; Demick, J. E.; Gautier, D.; Haberman, J. A.; Harpold, D. N.; Kasprzak, W. T.; Lunine, J. I.; Owen, T. C.; Raulin, F.

2010-01-01

The Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer (GCMS) determined the composition of the Titan atmosphere from 140km altitude to the surface. After landing, it returned composition data of gases evaporated from the surface. Height profiles of molecular nitrogen (N2), methane (CH4) and molecular hydrogen (H2) were determined. Traces were detected on the surface of evaporating methane, ethane (C2H6), acetylene (C2H2), cyanogen (C2N2) and carbon dioxide (CO2). The methane data showed evidence that methane precipitation occurred recently. The methane mole fraction was (1.48+/-0.09) x 10(exp -2) in the lower stratosphere (139.8 km to 75.5 km) and (5.65+/-0.18) x 10(exp -2) near the surface (6.7 km to the surface). The molecular hydrogen mole fraction was (1.01+/-0.16) x 10(exp -3) in the atmosphere and (9.90+/-0.17) x 10(exp -4) on the surface. Isotope ratios were 167.7+/-0.6 for N-14/N-15 in molecular nitrogen, 91.1+/-1.4 for C-12/C-13 in methane and (1.35+/-0.30) x 10(exp -4) for D/H in molecular hydrogen. The mole fractions of Ar-36 and radiogenic Ar-40 are (2.1+/-0.8) x 10(exp -7) and (3.39 +/-0.12) x 10(exp -5) respectively. Ne-22 has been tentatively identified at a mole fraction of (2.8+/-2.1) x 10(exp -7) Krypton and xenon were below the detection threshold of 1 x 10(exp -8) mole fraction. Science data were not retrieved from the gas chromatograph subsystem as the abundance of the organic trace gases in the atmosphere and on the ground did not reach the detection threshold. Results previously published from the GCMS experiment are superseded by this publication.

Liquid-phase chromatography detector

DOEpatents

Voigtman, Edward G.; Winefordner, James D.; Jurgensen, Arthur R.

1983-01-01

A liquid-phase chromatography detector comprising a flow cell having an inlet tubular conduit for receiving a liquid chromatographic effluent and discharging it as a flowing columnar stream onto a vertically adjustable receiving surface spaced apart from and located vertically below and in close proximity to the discharge end of the tubular conduit; a receiver adapted to receive liquid overflowing from the receiving surface; an exit conduit for continuously removing liquid from the receiver; a light source for focussing fluorescence-producing light pulses on the flowing columnar stream as it passes from the outlet of the conduit to the receiving surface and a fluorescence detector to detect the produced fluorescence; a source of light pulse for producing acoustic waves in the columnar stream as it passes from the conduit outlet to the receiving surface; and a piezoelectric transducer adapted to detect those waves; and a source of bias voltage applied to the inlet tubular conduit and adapted to produce ionization of the liquid flowing through the flow cell so as to produce photocurrents therein and an electrical system to detect and record the photocurrents. This system is useful in separating and detecting individual chemical compounds from mixtures thereof.

Gas chromatograph sample-transfer valve

NASA Technical Reports Server (NTRS)

Wang, W. S.; Wright, H. W., Jr.

1971-01-01

Slide-type gate valve incorporates sampling volume and transfer passageway for guiding a metered quantity of gas from pressurized test cell to gas chromatograph. Gate is moved by pneumatic bellows-type actuator.

Quantification of urinary uric acid in the presence of thymol and thimerosal by high-performance liquid chromatography

NASA Technical Reports Server (NTRS)

Chen, Y.; Pietrzyk, R. A.; Whitson, P. A.

1997-01-01

A high-performance liquid chromatographic method was developed as an alternative to automated enzymatic analysis of uric acid in human urine preserved with thymol and/or thimerosal. Uric acid (tR = 10 min) and creatinine (tR = 5 min) were separated and quantified during isocratic elution (0.025 M acetate buffer, pH 4.5) from a mu Bondapak C18 column. The uric-acid peak was identified chemically by incubating urine samples with uricase. The thymol/thimerosal peak appeared at 31 min during the washing step and did not interfere with the analysis. We validated the high-performance liquid chromatographic method for linearity, precision and accuracy, and the results were found to be excellent.

Simultaneous determination of primary and secondary phenethylamines in biological samples by high-performance liquid chromatographic method with fluorescence detection.

PubMed

Guo, Xiao-Feng; Wang, Jie-Yu; Wang, Hong; Zhang, Hua-Shan

2014-09-15

Phenylalanine is an essential amino acid and its metabolites relate to various physiological and immune functions of living organisms. To monitor the alteration of concentration of primary and secondary phenethylamines including N-methyltyramine, octopamine, tyramine, tyrosine and phenylalanine in the metabolic pathway of phenylalanine, a sensitive and selective reversed-phase high-performance liquid chromatographic method has been developed in this study. The identification and quantification of phenethylamines were performed by fluorescent detection after pre-column derivatization with 1,3,5,7-tetramethyl-8-(N-hydroxysuccinimidyl butyric ester)difluoroboradiaza-s-indacene, an excellent fluorescent probe which could react with both primary and secondary amino groups simultaneously. The derivatization was carried out at 25 °C for 25 min, and the separation was performed on a C18 column within 20 min. The linear ranges were from 2.0 to 100 nM for phenylalanine and tyramine to 5.0 to 250 for tyrosine and octopamine, with the detection limits of 0.1 nM for octopamine, tyramine, tyrosine and phenylalanine and 0.2 nM for N-methyltyramine (signal-to-noise ratio=3), which allowed for the sure determination of phenethylamines at trace levels in the real samples without complex pretreatment or enrichment during multitudinous samples analysis. The proposed method has been validated by the analysis of the five target compounds in biological samples with spiked recoveries of 96.4-104.4% and the relative standard deviation of 1.0 and 4.4%. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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.

Studies on Chromatographic Fingerprint and Fingerprinting Profile-Efficacy Relationship of Polygoni Perfoliati Herba

PubMed Central

Tian, Li; Chen, Hua-Guo; Zhao, Chao; Gong, Xiao-Jian

2013-01-01

Polygoni Perfoliati Herba is widely used in China with antibacterium, anti-inflammatory, expectorant, antitumor, and antivirus activities. To reveal the mechanisms of the activities of Polygoni Perfoliati Herba, the relationship between the fingerprinting profile and its bioactivities was investigated. In the present study, high-performance liquid chromatographic (HPLC) fingerprinting method was developed. The established method was applied to analyze 51 batches of Polygoni Perfoliati Herba samples collected from different locations or in different harvesting times in China. Chemometrics, including similarity analysis, hierarchical clustering analysis, and principal component analysis, were used to express their similarities. It was found that similarity values of the samples were in the range of 0.432–0.998. The results of analgesic tests indicated that Polygoni Perfoliati Herba could significantly inhibit pain induced by hot plate and acetic acid in mice. The results of anti-inflammatory tests showed that Polygoni Perfoliati Herba had good anti-inflammatory effects (P < 0.01) in two models including dimethyl benzene-induced ear edema and acetic acid-induced peritoneal permeability in mice. Combining the results from chromatographic fingerprints with those from bioactivities, we found that seven peaks from Polygoni Perfoliati Herba were mainly responsible for analgesic and anti-inflammatory activities. PMID:24023580

Optimisation and validation of a rapid and efficient microemulsion liquid chromatographic (MELC) method for the determination of paracetamol (acetaminophen) content in a suppository formulation.

PubMed

McEvoy, Eamon; Donegan, Sheila; Power, Joe; Altria, Kevin

2007-05-09

A rapid and efficient oil-in-water microemulsion liquid chromatographic method has been optimised and validated for the analysis of paracetamol in a suppository formulation. Excellent linearity, accuracy, precision and assay results were obtained. Lengthy sample pre-treatment/extraction procedures were eliminated due to the solubilising power of the microemulsion and rapid analysis times were achieved. The method was optimised to achieve rapid analysis time and relatively high peak efficiencies. A standard microemulsion composition of 33 g SDS, 66 g butan-1-ol, 8 g n-octane in 1l of 0.05% TFA modified with acetonitrile has been shown to be suitable for the rapid analysis of paracetamol in highly hydrophobic preparations under isocratic conditions. Validated assay results and overall analysis time of the optimised method was compared to British Pharmacopoeia reference methods. Sample preparation and analysis times for the MELC analysis of paracetamol in a suppository were extremely rapid compared to the reference method and similar assay results were achieved. A gradient MELC method using the same microemulsion has been optimised for the resolution of paracetamol and five of its related substances in approximately 7 min.

Effect of Impurities on the Triple Point of Water: Experiments with Doped Cells at Different Liquid Fractions

NASA Astrophysics Data System (ADS)

Dobre, M.; Peruzzi, A.; Kalemci, M.; Van Geel, J.; Maeck, M.; Uytun, A.

2018-05-01

Recent international comparisons showed that there is still room for improvement in triple point of water (TPW) realization uncertainty. Large groups of cells manufactured, maintained and measured in similar conditions still show a spread in the realized TPW temperature that is larger than the best measurement uncertainties (25 µK). One cause is the time-dependent concentration of dissolved impurities in water. The origin of such impurities is the glass/quartz envelope dissolution during a cell lifetime. The effect is a difference in the triple point temperature proportional to the impurities concentration. In order to measure this temperature difference and to investigate the effect of different types of impurities, we manufactured doped cells with different concentrations of silicon (Si), boron (B), sodium (Na) and potassium (K), the glass main chemical components. To identify any influence of the filling process, two completely independent manufacturing procedures were followed in two different laboratories, both national metrology institutes (VSL, Netherlands and UME, Turkey). Cells glass and filling water were also different while the doping materials were identical. Measuring the temperature difference as a function of the liquid fraction is a method to obtain information about impurities concentrations in TPW. Only cells doped with 1 µmol·mol-1 B, Na and K proved to be suitable for measurements at different liquid fractions. We present here the results with related uncertainties and discuss the critical points in this experimental approach.

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

PubMed

Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

2017-09-01

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

19 CFR 159.3 - Rounding of fractions.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 19 Customs Duties 2 2010-04-01 2010-04-01 false Rounding of fractions. 159.3 Section 159.3 Customs... (CONTINUED) LIQUIDATION OF DUTIES General Provisions § 159.3 Rounding of fractions. (a) Value. In the... cents or more, the lower fractions shall be dropped, and if it is necessary to take up as whole dollars...

Extraction of ranitidine and nizatidine with using imidazolium ionic liquids prior spectrophotometric and chromatographic detection.

PubMed

Kiszkiel, Ilona; Starczewska, Barbara; Leśniewska, Barbara; Późniak, Patrycja

2015-03-15

A new extraction medium was proposed for liquid-liquid extraction of the histamine H2 receptor antagonists ranitidine (RNT) and nizatidine (NZT). The ionic liquids with low vapor pressure and favorable solvating properties for a range of compounds such as 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] and 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide [C4mim][Tf2N] were tested for isolation of analytes. The extraction parameters of RNT and NZT, namely, amount of ionic liquid, pH of sample solution, shaking and centrifugation time were optimized. The isolation processes were performed with 1 mL of the ionic liquids. The extracted samples (pH values near 4) were shaken at 1750 rpm. The influence of interfering substances on the efficiency of extraction process was also studied. Methods for the histamine H2 receptor antagonists (ranitidine and nizatidine) determination after their separation using imidazolium ionic liquids by high performance liquid chromatography (HPLC) combined with UV spectrophotometry were developed. The application of ionic liquids in extraction step allows for selective isolation of analytes from aqueous matrices and their preconcentration. The above methods were applied to the determination of RNT and NZT in environmental samples (river water and wastewater after treatment). Copyright © 2014 Elsevier B.V. All rights reserved.

Additional band broadening of peptides in the first size-exclusion chromatographic dimension of an automated stop-flow two-dimensional high performance liquid chromatography.

PubMed

Xu, Jucai; Sun-Waterhouse, Dongxiao; Qiu, Chaoying; Zhao, Mouming; Sun, Baoguo; Lin, Lianzhu; Su, Guowan

2017-10-27

The need to improve the peak capacity of liquid chromatography motivates the development of two-dimensional analysis systems. This paper presented a fully automated stop-flow two-dimensional liquid chromatography system with size exclusion chromatography followed by reversed phase liquid chromatography (SEC×RPLC) to efficiently separate peptides. The effects of different stop-flow operational parameters (stop-flow time, peak parking position, number of stop-flow periods and column temperature) on band broadening in the first dimension (1 st D) SEC column were quantitatively evaluated by using commercial small proteins and peptides. Results showed that the effects of peak parking position and the number of stop-flow periods on band broadening were relatively small. Unlike stop-flow analysis of large molecules with a long running time, additional band broadening was evidently observed for small molecule analytes due to the relatively high effective diffusion coefficient (D eff ). Therefore, shorter analysis time and lower 1 st D column temperature were suggested for analyzing small molecules. The stop-flow two-dimensional liquid chromatography (2D-LC) system was further tested on peanut peptides and an evidently improved resolution was observed for both stop-flow heart-cutting and comprehensive 2D-LC analysis (in spite of additional band broadening in SEC). The stop-flow SEC×RPLC, especially heart-cutting analysis with shorter analysis time and higher 1 st D resolution for selected fractions, offers a promising approach for efficient analysis of complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Taste and chemical characteristics of low molecular weight fractions from tofuyo - Japanese fermented soybean curd.

PubMed

Lioe, Hanifah Nuryani; Kinjo, Ayano; Yasuda, Shin; Kuba-Miyara, Megumi; Tachibana, Shinjiro; Yasuda, Masaaki

2018-06-30

Tofuyo, a Japanese traditional food, is a fermented soybean curd manufactured in Okinawa region. Due to its original cheese-like flavor, the current study was designed to evaluate the sensory and chemical characteristics of three stepwise ultrafiltration fractions, using 10,000, 3000 and 500 Da membranes and further chromatographic fractions from tofuyo. The results showed that umami, sweet and salty were the characteristic tastes of all fractions, with umami intensity evaluated for the fraction with MW less than 500 Da (F-500) as the most prominent among the three fractions. Subsequent Sephadex G-25 SF fractions and RP-HPLC fractions were subjected to sensory and chemical analyses. The tastiest fraction contained sodium chloride, sugars, organic acids, umami and sweet free amino acids, at concentrations above their thresholds. The abundant presence of umami and sweet free amino acids with certain concentrations of sodium chloride and glucose might provide the typical savory taste of tofuyo. Copyright © 2018 Elsevier Ltd. All rights reserved.

Determination of noscapine, hexylresorcinol and anethole in cough lozenges by liquid chromatography.

PubMed

Lucangioli, S; Fernández Otero, G; Rodríguez, V; Carducci, C N

1996-06-01

A liquid chromatographic method was developed for the simultaneous separation and determination of noscapine hydrochloride, hexylresorcinol and anethole in cough lozenges. Analysis was performed on a phenyl column with phosphate buffer- acetonitrile as mobile phase and the separated components were detected at 282 mm. Recoveries obtained for the analytes were of 94.6% for noscapine hydrochloride, 99.1% for hexylresorcinol and 96.3% for anethole. The values of the relative standard deviation were 0.8% for noscapine hydrochloride, 1.5% for hexylresorcinol and 1.1% for anethole. The analytical method was validated and a system suitability test was accomplished for the chromatographic method.

Liquid chromatography/mass spectrometry and liquid chromatography/nuclear magnetic resonance as complementary analytical techniques for unambiguous identification of polymethoxylated flavones in residues from molecular distillation of orange peel oils (Citrus sinensis).

PubMed

Weber, Berthold; Hartmann, Beate; Stöckigt, Detlef; Schreiber, Klaus; Roloff, Michael; Bertram, Heinz-Jürgen; Schmidt, Claus O

2006-01-25

Liquid chromatography/mass spectrometry and liquid chromatography/nuclear magnetic resonance techniques with ultraviolet/diode array detection were used as complementary analytical tools for the reliable identification of polymethoxylated flavones in residues from molecular distillation of cold-pressed peel oils of Citrus sinensis. After development of a liquid chromatographic separation procedure, the presence of several polymethoxy flavones such as sinensetin, nobiletin, tangeretin, quercetogetin, heptamethoxyflavone, and other derivatives was unambiguously confirmed. In addition, proceranone, an acetylated tetranortriterpenoid with limonoid structure, was identified for the first time in citrus.

Inorganic selenium speciation analysis in Allium and Brassica vegetables by ionic liquid assisted liquid-liquid microextraction with multivariate optimization.

PubMed

Castro Grijalba, Alexander; Martinis, Estefanía M; Wuilloud, Rodolfo G

2017-03-15

A highly sensitive vortex assisted liquid-liquid microextraction (VA-LLME) method was developed for inorganic Se [Se(IV) and Se(VI)] speciation analysis in Allium and Brassica vegetables. Trihexyl(tetradecyl)phosphonium decanoate phosphonium ionic liquid (IL) was applied for the extraction of Se(IV)-ammonium pyrrolidine dithiocarbamate (APDC) complex followed by Se determination with electrothermal atomic absorption spectrometry. A complete optimization of the graphite furnace temperature program was developed for accurate determination of Se in the IL-enriched extracts and multivariate statistical optimization was performed to define the conditions for the highest extraction efficiency. Significant factors of IL-VA-LLME method were sample volume, extraction pH, extraction time and APDC concentration. High extraction efficiency (90%), a 100-fold preconcentration factor and a detection limit of 5.0ng/L were achieved. The high sensitivity obtained with preconcentration and the non-chromatographic separation of inorganic Se species in complex matrix samples such as garlic, onion, leek, broccoli and cauliflower, are the main advantages of IL-VA-LLME. Copyright © 2016 Elsevier Ltd. All rights reserved.

Rational and Efficient Preparative Isolation of Natural Products by MPLC-UV-ELSD based on HPLC to MPLC Gradient Transfer.

PubMed

Challal, Soura; Queiroz, Emerson Ferreira; Debrus, Benjamin; Kloeti, Werner; Guillarme, Davy; Gupta, Mahabir Prashad; Wolfender, Jean-Luc

2015-11-01

In natural product research, the isolation of biomarkers or bioactive compounds from complex natural extracts represents an essential step for de novo identification and bioactivity assessment. When pure natural products have to be obtained in milligram quantities, the chromatographic steps are generally labourious and time-consuming. In this respect, an efficient method has been developed for the reversed-phase gradient transfer from high-performance liquid chromatography to medium-performance liquid chromatography for the isolation of pure natural products at the level of tens of milligrams from complex crude natural extracts. The proposed method provides a rational way to predict retention behaviour and resolution at the analytical scale prior to medium-performance liquid chromatography, and guarantees similar performances at both analytical and preparative scales. The optimisation of the high-performance liquid chromatography separation and system characterisation allows for the prediction of the gradient at the medium-performance liquid chromatography scale by using identical stationary phase chemistries. The samples were introduced in medium-performance liquid chromatography using a pressure-resistant aluminium dry load cell especially designed for this study to allow high sample loading while maintaining a maximum achievable flow rate for the separation. The method has been validated with a mixture of eight natural product standards. Ultraviolet and evaporative light scattering detections were used in parallel for a comprehensive monitoring. In addition, post-chromatographic mass spectrometry detection was provided by high-throughput ultrahigh-performance liquid chromatography time-of-flight mass spectrometry analyses of all fractions. The processing of all liquid chromatography-mass spectrometry data in the form of an medium-performance liquid chromatography x ultra high-performance liquid chromatography time-of-flight mass spectrometry matrix enabled an

Combined liquid chromatography-mass spectrometry for trace analysis of pharmaceuticals

NASA Astrophysics Data System (ADS)

Schmidt, Lothar; Danigel, Harald; Jungclas, Hartmut

1982-07-01

A 252Cf-plasma desorption mass spectrometer (PDMS) for the analysis of thin layers from nonvolatile organic samples has been set up to be combined with a liquid chromatograph. A novel interface performs the direct inlet of the liquid sample through a capillary into the vacuum system of the spectrometer. Samples of drugs are periodically collected, transferred to the ion source and analysed using a rotating disk. This on-line sample preparation has been tested for three antiarrhythmic drugs using various solvents and mixtures.

Mesophilic anaerobic co-digestion of the organic fraction of municipal solid waste with the liquid fraction from hydrothermal carbonization of sewage sludge.

PubMed

De la Rubia, M A; Villamil, J A; Rodriguez, J J; Borja, R; Mohedano, A F

2018-06-01

In the present study, the influence of substrate pre-treatment (grinding and sieving) on batch anaerobic digestion of the organic fraction of municipal solid waste (OFMSW) was first assessed, then followed by co-digestion experiments with the liquid fraction from hydrothermal carbonization (LFHTC) of dewatered sewage sludge (DSS). The methane yield of batch anaerobic digestion after grinding and sieving (20 mm diameter) the OFMSW was considerably higher (453 mL CH 4 STP g -1 VS added ) than that of untreated OFMSW (285 mL CH 4 STP g -1 VS added ). The modified Gompertz model adequately predicted process performance. The maximum methane production rate, R m , for ground and sieved OFMSW was 2.4 times higher than that of untreated OFMSW. The anaerobic co-digestion of different mixtures of OFMSW and LFHTC of DSS did not increase the methane yield above that of the anaerobic digestion of OFMSW alone, and no synergistic effects were observed. However, the co-digestion of both wastes at a ratio of 75% OFMSW-25% LFHTC provides a practical waste management option. The experimental results were adequately fitted to a first-order kinetic model showing a kinetic constant virtually independent of the percentage of LFHTC (0.52-0.56 d -1 ) and decreasing slightly for 100% LFHTC (0.44 d -1 ). Copyright © 2018 Elsevier Ltd. All rights reserved.

Quantification of nitrogen in the liquid fraction and in vitro assessment of lysine bioavailability in the solid fraction of soybean meal hydrolysates.

PubMed

Luján-Rhenals, D; Morawicki, R; Shi, Z; Ricke, S C

2018-01-02

Soybean meal (SBM) is a product generated from the manufacture of soybean oil and has the potential for use as a source of fermentable sugars for ethanol production or as a protein source for animal feeds. Knowing the levels of nitrogen available from ammonium is a necessary element of the ethanolic fermentation process while identifying the levels of essential amino acids such as lysine is important in determining usage as a feed source. As such the purpose of this study was to quantify total nitrogen and ammonium in the liquid fraction of hydrolyzed SBM and to evaluate total and bioavailable lysine in the solid fraction of the hydrolyzed SBM. The effects of acid concentration, cellulase and β-glucosidase on total and ammonium nitrogen were studied with analysis indicating that higher acid concentrations increased nitrogen compounds with ammonium concentrations ranging from 0.20 to 1.24 g L -1 while enzymatic treatments did not significantly increase nitrogen levels. Total and bioavailable lysine was quantified by use of an auxotrophic gfpmut3 E.coli whole-cell bioassay organism incapable of lysine biosynthesis. Acid and enzymatic treatments were applied with lysine bioavailability increasing from a base of 82% for untreated SBM to up to 97%. Our results demonstrated that SBM has the potential to serve in ethanolic fermentation and as an optimal source essential amino acid lysine.

Fabrication of an ionic-liquid-based polymer monolithic column and its application in the fractionation of proteins from complex biosamples.

PubMed

Zhang, Doudou; Zhang, Qian; Bai, Ligai; Han, Dandan; Liu, Haiyan; Yan, Hongyuan

2018-05-01

An ionic-liquid-based polymer monolithic column was synthesized by free radical polymerization within the confines of a stainless-steel column (50 mm × 4.6 mm id). In the processes, ionic liquid and stearyl methacrylate were used as dual monomers, ethylene glycol dimethacrylate as the cross-linking agent, and polyethylene glycol 200 and isopropanol as co-porogens. Effects of the prepolymerization solution components on the properties of the resulting monoliths were studied in detail. Scanning electron microscopy, nitrogen adsorption-desorption measurements, and mercury intrusion porosimetry were used to investigate the morphology and pore size distribution of the prepared monoliths, which showed that the homemade ionic-liquid-based monolith column possessed a relatively uniform macropore structure with a total macropore specific surface area of 44.72 m 2 /g. Compared to a non-ionic-liquid-based monolith prepared under the same conditions, the ionic-liquid-based monolith exhibited excellent selectivity and high performance for separating proteins from complex biosamples, such as egg white, snailase, bovine serum albumin digest solution, human plasma, etc., indicating promising applications in the fractionation and analysis of proteins from the complex biosamples in proteomics research. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Authenticity analysis of pear juice employing chromatographic fingerprinting.

PubMed

Willems, Jamie L; Low, Nicholas H

2014-12-03

Pear juice is predominately composed of carbohydrates/polyols (>95% of the total soluble solids), making it susceptible to adulteration by the addition of less expensive commercial sweeteners. In this research, the major carbohydrate and polyol (fructose, glucose, sucrose, and sorbitol) content of 32 pure pear juices representing five world producing regions and three years of production was determined. Additionally, methods employing oligosaccharide profiling to detect the debasing of these samples with four commercial sweeteners (HFCS 55 and 90, TIS, and HIS) were developed using capillary gas chromatography with flame ionization detection (CGC-FID) and high-performance liquid chromatography with pulsed amperometric detection (HPAE-PAD). Detection limits for the four commercial sweeteners ranged from 0.5 to 5.0% (v/v). In addition, the developed CGC-FID method could be used to (a) detect the addition of pear to apple juice via arbutin detection and (b) determine if a pear juice was produced using enzymatic liquefaction via the presence of O-β-d-glucopyranosyl-(1→4)-d-glucopyranose (cellobiose), all within a single chromatographic analysis.

Void fraction development in gas-liquid flow after a U-bend in a vertically upwards serpentine-configuration large-diameter pipe

NASA Astrophysics Data System (ADS)

Almabrok, Almabrok A.; Aliyu, Aliyu M.; Baba, Yahaya D.; Lao, Liyun; Yeung, Hoi

2018-01-01

We investigate the effect of a return U-bend on flow behaviour in the vertical upward section of a large-diameter pipe. A wire mesh sensor was employed to study the void fraction distributions at axial distances of 5, 28 and 47 pipe diameters after the upstream bottom bend. The study found that, the bottom bend has considerable impacts on up-flow behaviour. In all conditions, centrifugal action causes appreciable misdistribution in the adjacent straight section. Plots from WMS measurements show that flow asymmetry significantly reduces along the axis at L/D = 47. Regime maps generated from three axial locations showed that, in addition to bubbly, intermittent and annular flows, oscillatory flow occurred particularly when gas and liquid flow rates were relatively low. At this position, mean void fractions were in agreement with those from other large-pipe studies, and comparisons were made with existing void fraction correlations. Among the correlations surveyed, drift flux-type correlations were found to give the best predictive results.

Influence of a strong sample solvent on analyte dispersion in chromatographic columns.

PubMed

Mishra, Manoranjan; Rana, Chinar; De Wit, A; Martin, Michel

2013-07-05

In chromatographic columns, when the eluting strength of the sample solvent is larger than that of the carrier liquid, a deformation of the analyte zone occurs because its frontal part moves at a relatively high velocity due to a low retention factor in the sample solvent while the rear part of the analyte zone is more retained in the carrier liquid and hence moves at a lower velocity. The influence of this solvent strength effect on the separation of analytes is studied here theoretically using a mass balance model describing the spatio-temporal evolution of the eluent, the sample solvent and the analyte. The viscosity of the sample solvent and carrier fluid is supposed to be the same (i.e. no viscous fingering effects are taken into account). A linear isotherm adsorption with a retention factor depending upon the local concentration of the liquid phase is considered. The governing equations are numerically solved by using a Fourier spectral method and parametric studies are performed to analyze the effect of various governing parameters on the dispersion and skewness of the analyte zone. The distortion of this zone is found to depend strongly on the difference in eluting strength between the mobile phase and the sample solvent as well as on the sample volume. Copyright © 2013 Elsevier B.V. All rights reserved.

Low-level (PPB) determination of cisplatin in cleaning validation (rinse water) samples. II. A high-performance liquid chromatographic method.

PubMed

Raghavan, R; Burchett, M; Loffredo, D; Mulligan, J A

2000-04-01

A high-performance liquid chromatographic (HPLC) method is described for the determination of residual levels of cisplatin from extracts of surfaces with very low surface area; from extracts of surfaces of coupons made of Teflon (polytetrafluoroethylene, PTFE), stainless steel, and glass; and in aqueous solution collected after rinsing equipment and parts. Initially, the method was developed to determine cisplatin at concentrations ranging from 20 to 200 ng/ml by direct injection. Retaining the same method conditions, the scope of the method was expanded by the addition of a sample preconcentration step, allowing analyses at levels ranging from 0.5 ng to 20 ng/ml. Preconcentration is necessary for the determination of cisplatin in rinse waters at a quantifiable concentration of about 2 PPB. Under these conditions, the detection limit is about 0.2 to 0.3 ng/ml. Residual cisplatin on different types of surfaces, including surfaces with very low surface area, can be determined by swabbing each test surface with a derivatizing solution. The cisplatin recovered in the swabbing solution can be analyzed by HPLC using direct injection or preconcentration, depending on the expected level of cisplatin in the sample. Initial methods were developed to quantitate at a cisplatin concentration of about 100 PPB or higher in solution extracted from surfaces. However, when surface areas are limited because of the size of the parts, solution concentration becomes very low as a result of the minimum volume required for extraction. To support the application of swabbing techniques to surface analysis, stainless steel, Teflon, and glass surfaces were spiked with cisplatin at 2.5 to 20 ng/cm2. Satisfactory overall recoveries of 90% +/- 10% were obtained from all surfaces. Cisplatin has no ultraviolet/visible (UV/Vis) spectral-active functional group that can be used to detect low levels of cisplatin. Hence, diethyldithiocarbamate (DDTC) was used as a derivatizing agent to increase

21 CFR 862.2230 - Chromatographic separation material for clinical use.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Chromatographic separation material for clinical... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory Instruments § 862.2230 Chromatographic separation material for clinical use. (a) Identification. A...

Fundamental studies of chalcogenide nanocrystals, carbonaceous nanoparticles, and chromatographic materials

NASA Astrophysics Data System (ADS)

Baker, Jared Scott

2011-12-01

electrophoretic mobilities under a wide range of pH values. The mobility of these nanoparticles as a function of ionic strength was compared to classical electrokinetic theory, suggesting that the species are small, highly charged particles with appreciable zeta potentials, even at low pH. In an attempt to reduce the complexity of the CNP solution, two molecular-weight based fractionation techniques were employed and evaluated. Traditional dialysis and ultracentrifugation filtration techniques were modified to generate multiple CNPs fractions based on size. Analysis of the fractions by absorption and photoluminescence spectroscopy as well as CE revealed specific characteristics for a given sized-fraction. Namely, a strong correlation between the size of the CNPs and their luminescent emission was observed. CE was utilized to characterize each fraction and to ultimately judge the effectiveness of the fractionation techniques. The characterization of the persistence and degradation of magic-sized CdSe nanocrystals (NCs) after their removal from the original reaction mixture and dispersion into basic aqueous solutions was performed by absorption spectroscopy. NCs degraded after dilution into aqueous NaOH, resulting in red-shifted excitonic absorption bands and eventual flocculation. Dilution of NCs into basic aqueous solutions of cysteinate resulted in degradation via a different mechanism with an absence of flocculation; kinetics varied with concentration of cysteinate. The chemical fate of NCs after dilution into basic aqueous solutions containing both Cd2+ and cysteinate varied with the cysteinate-to-Cd 2+ molar ratio, which determined the relative solute mole fractions of various Cd2+-cysteinate complexes. CdSe NCs persisted on long timescales only when dispersed in solutions containing [Cd(cysteinate) 3]4-. Equilibria are presented to account for the observed spectral changes after dilution of CdSe into various basic media. Cadmium(II)-cysteinate complex-formation equilibria

Separation of silver nanoparticles by hollow fiber flow field-flow fractionation: Addition of tannic acid into carrier liquid as a modifier.

PubMed

Saenmuangchin, Rattaporn; Mettakoonpitak, Jaruwan; Shiowatana, Juwadee; Siripinyanond, Atitaya

2015-10-09

A homemade hollow fiber flow-field fractionation (Hf-FlFFF) coupled with inductively coupled plasma mass spectrometry (ICP-MS) was set-up for silver nanoparticles (AgNPs) separation by using polysulfone hollow fiber membrane (30,000 MW cutoff) as a separation channel. Tannic acid and citrate stabilized AgNPs were synthesized and introduced into Hf-FlFFF. The effects of carrier liquid and stabilizing agent on retention behavior of AgNPs were investigated. Different elution behaviors were observed as follows: with 0.02% (w/v) FL-70, all of AgNPs were eluted from Hf-FlFFF but differences in retention behaviors were observed for AgNPs with tannic acid and citrate stabilizing agents; and with 30mM TRIS buffer, only tannic acid stabilized AgNPs were eluted from Hf-FlFFF, whereas citrate stabilized AgNPs were not eluted. In this work, tannic acid addition into carrier liquid was proposed to modify the surface of AgNPs and the surface of the membrane, and thereby adjusting the retention behaviors of AgNPs. Various concentrations of tannic acid were added into FL-70 and TRIS buffer. With the use of 0.1mM tannic acid in 30mM TRIS buffer as the carrier liquid, retention behaviors of both tannic acid stabilized- and citrate stabilized-AgNPs were similar and with similar fractionation recovery. Copyright © 2015 Elsevier B.V. All rights reserved.

To Flavor or Not to Flavor Extemporaneous Omeprazole Liquid.

PubMed

Chuong, Monica C; Taglieri, Catherine A; Kerr, Stephen G

2017-01-01

Omeprazole is a proton pump inhibitor used to treat the symptoms of gastro esophageal reflux disease, ulcers, excess stomach acid, infection with Helicobacter pylori, and to control the gastric side effects of various drugs. The approved dosage forms in the U.S. are powder in compounding kits, delayed-release granules for oral suspension, oral delayed-release tablets, and oral delayed-release capsules. An extemporaneously compounded unsweetened oral liquid method, published in the International Journal of Pharmaceutical Compounding, was found to be commonly used by pharmacists. This project investigated the robustness of the compendium omeprazole high-performance liquid chromatographic assay in evaluating an oral liquid made from commercial delayed-release pellets, the potency of extemporaneously compounded solutions having a 1.125% v/v flavored versus unflavored samples stored at controlled cold temperatures at different time points, and examining the absorption spectrum of the flavoring agent. As part of the study, stability-indication testing was also conducted. The studies indicate that the chromatographic area under the plasma concentration-time curve of both study groups remained over 90% of the label claim during the follow-up period. The flavor did not significantly impact the pH of the oral liquid. This study further identified (1) an increase in resilient foam formation in the flavored liquid, potentially hindering dosing accuracy, (2) omeprazole is oxidized easily by 3% hydrogen peroxide, and (3) flavoring agent absorbs in an ultraviolet visible spectroscopy spectral range often used in assay detectors for quantification of drug molecules, and could interfere with assay protocols of the same. Copyright© by International Journal of Pharmaceutical Compounding, Inc.

Capillary liquid chromatography combined with pressurized liquid extraction and dispersive liquid-liquid microextraction for the determination of vitamin E in cosmetic products.

PubMed

Viñas, Pilar; Pastor-Belda, Marta; Campillo, Natalia; Bravo-Bravo, María; Hernández-Córdoba, Manuel

2014-06-01

Capillary liquid chromatography (LC) is used for the determination of tocopherols and tocotrienols in cosmetic products. Dispersive liquid-liquid microextraction (DLLME) allows the analytes to be preconcentrated into a very small volume of organic solvent which is then injected into the chromatograph running at a very low flow rate. Pressurized liquid extraction (PLE) at a high temperature and pressure was used to isolate vitamin E forms from cosmetics. The Taguchi experimental method was used to optimize the factors affecting DLLME. The parameters selected were 2mL of acetonitrile (disperser solvent), 100μL carbon tetrachloride (extraction solvent) and 10mL aqueous solution. A volume of 5μL of the organic phase was injected into the reversed-phase capillary LC system equipped with a diode array detector and using an isocratic mobile phase composed of an 95:5 (v/v) methanol:water mixture at a flow-rate of 20μLmin(-1). Quantification was carried out using aqueous standards and detection limits were in the range 0.1-0.5ngmL(-1), corresponding to 3-15ngg(-1) in the cosmetic sample. The recoveries were in the 87-105% range, with RSDs lower than 7.8%. The method was validated according to international guidelines and using a certified reference material. Copyright © 2014 Elsevier B.V. All rights reserved.

Enantiomeric fraction of styrene glycol as a biomarker of occupational risk exposure to styrene.

PubMed

Lima, J J; Aguilar, A; Sánchez, F G; Díaz, A N

2017-02-01

This work reports a new analytical approach for monitoring the enantiomeric ratios of styrene glycol (SG), encountered during the manufacture of plastics, by chiral liquid chromatography and the application as a biomarker for exposure to styrene. The isomers were separated using an AGP column running in the reverse phase and isocratic mode with a mobile phase consisting of 20 mM phosphate buffer saline (pH 4.15) and methanol at a flow rate of 0.8 mL/min. Photometric, polarimetric, and circular dichroism detectors were employed. The chromatographic enantioselective resolution (Rs) and selectivity index (α) values were determined to be 1.60 and 1.48 (by photometric detection), respectively. Calibration curves used for the quantification of the SG enantiomers were linear with a correlation coefficient >0.99; the detection limits were in the range of 0.03-0.16 μg, depending on the detector used. Recovery assays on synthetic samples (in triplicate) covering the full range of enantiomeric fractions (0.0-1.0) show accuracy values below 5% for the enantiomeric fraction (EF) in every case. An alternative method based on the measurement of anisotropy factors for the determination of EF, which is faster and does not require the separation of enantiomers, has also been developed. The enantiomeric excess of the toxicant biomarker styrene glycol has been determined. No previous direct enantioselective determination of styrene glycol was published. Copyright © 2016 Elsevier Ltd. All rights reserved.

A simple high-performance liquid chromatographic method for the determination of acyclovir in human plasma and application to a pharmacokinetic study.

PubMed

Yu, Liyan; Xiang, Bingren; Zhan, Ying

2008-01-01

A rapid, simple and sensitive reversed-phase high-performance liquid chromatographic (HPLC) method has been developed for the measurement of acyclovir (CAS 59277-89-3) concentrations in human plasma and its use in bioavailability studies is evaluated. The method was linear in the concentration range of 0.05-4.0 microg/ml. The lower limit of quantification (LLOQ) was 0.05 microg/ml in 0.5 ml plasma sample. The intra- and inter-day relative standard deviations across three validation runs over the entire concentration range were less than 8.2%. This method was successfully applied for the evaluation of pharmacokinetic profiles of acyclovir capsule in 19 healthy volunteers. The main pharmacokinetic parameters obtained were: AUC(o-t) 6.50 +/- 1.47 and 7.13 +/- 1.44 microg x h/ml, AUC(0-infinity) 6.77 +/- 1.48 and 7.41 +/- 1.49 microg x h/ml, C(max) 2.27 +/- 0.57 and 2.27 +/- 0.62 microg/ml, t(1/2) 2.96 +/- 0.41 and 2.88 +/- 0.33 h, t(max) 0.8 +/- 0.3 and 1.0 +/- 0.5 h for test and reference formulations, respectively. No statistical differences were observed for C(max) and the area under the plasma concentration--time curve for acyclovir. 90% confidence limits calculated for C(max) and AUC from zero to infinity (AUC(0-infinity)) of acyclovir were included in the bioequivalence range (0.8-1.25 for AUC).

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

PubMed

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.

Optimized and validated high-performance liquid chromatography method for the determination of deoxynivalenol and aflatoxins in cereals.

PubMed

Skendi, Adriana; Irakli, Maria N; Papageorgiou, Maria D

2016-04-01

A simple, sensitive and accurate analytical method was optimized and developed for the determination of deoxynivalenol and aflatoxins in cereals intended for human consumption using high-performance liquid chromatography with diode array and fluorescence detection and a photochemical reactor for enhanced detection. A response surface methodology, using a fractional central composite design, was carried out for optimization of the water percentage at the beginning of the run (X1, 80-90%), the level of acetonitrile at the end of gradient system (X2, 10-20%) with the water percentage fixed at 60%, and the flow rate (X3, 0.8-1.2 mL/min). The studied responses were the chromatographic peak area, the resolution factor and the time of analysis. Optimal chromatographic conditions were: X1 = 80%, X2 = 10%, and X3 = 1 mL/min. Following a double sample extraction with water and a mixture of methanol/water, mycotoxins were rapidly purified by an optimized solid-phase extraction protocol. The optimized method was further validated with respect to linearity (R(2) >0.9991), sensitivity, precision, and recovery (90-112%). The application to 23 commercial cereal samples from Greece showed contamination levels below the legally set limits, except for one maize sample. The main advantages of the developed method are the simplicity of operation and the low cost. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HOT ELUENT CAPILLARY LIQUID CHROMATOGRAPHY USING ZIRCONIA AND TITANIA BASED STATIONARY PHASES. (R825344)

EPA Science Inventory

Abstract

High speed capillary liquid chromatographic separations using a simple home made system constructed from readily available inexpensive components have been studied. Using thermally stable zirconia and titania based packing, the separation of eight alkylbenzene...

Liquid-phase chromatography detector

DOEpatents

Voigtman, E.G.; Winefordner, J.D.; Jurgensen, A.R.

1983-11-08

A liquid-phase chromatography detector comprises a flow cell having an inlet tubular conduit for receiving a liquid chromatographic effluent and discharging it as a flowing columnar stream onto a vertically adjustable receiving surface spaced apart from and located vertically below and in close proximity to the discharge end of the tubular conduit; a receiver adapted to receive liquid overflowing from the receiving surface; an exit conduit for continuously removing liquid from the receiver; a light source for focusing fluorescence-producing light pulses on the flowing columnar stream as it passes from the outlet of the conduit to the receiving surface and a fluorescence detector to detect the produced fluorescence; a source of light pulse for producing acoustic waves in the columnar stream as it passes from the conduit outlet to the receiving surface; and a piezoelectric transducer adapted to detect those waves; and a source of bias voltage applied to the inlet tubular conduit and adapted to produce ionization of the liquid flowing through the flow cell so as to produce photocurrents therein and an electrical system to detect and record the photocurrents. This system is useful in separating and detecting individual chemical compounds from mixtures thereof. 5 figs.

Comparison of the ion exclusion chromatographic method with the Monier-Williams method for determination of total sulfite in foods.

PubMed

Kim, H J

1989-01-01

Experimental data comparing the alkali extraction/ion exclusion chromatographic method with the Monier-Williams method for determination of total sulfite are presented in (a) enzymatic and nonenzymatic browning systems, (b) vegetables containing naturally occurring sulfite, and (c) a carbohydrate-type food additive, erythorbic acid. Excellent agreement, with a linear correlation coefficient of 0.99, was observed in fresh potato samples homogenized with sulfite and allowed to react for different time intervals (enzymatic browning system). A good overall correlation was observed in dehydrated, sulfited apple samples heated for different times (nonenzymatic browning system); however, as heating time increased, higher results were obtained by the Monier-Williams method than by the alkali extraction/ion exclusion chromatographic method. The results of determining sulfite in the alkali trapping solution following acid distillation or acid treatment without heat suggested that this deviation was due to a fraction of sulfite bound to the browning reaction products in such a way that it was released by acid distillation but not by alkali extraction or acid treatment without heat. Similar behavior was demonstrated in cabbage with naturally occurring sulfite, which was released by acid distillation but not by alkali extraction or acid treatment without heat. The ion exclusion chromatographic method could overcome interference by the volatile caramelization reaction products in the Monier-Williams determination of erythorbic acid.

Piper betel leaf extract: anticancer benefits and bio-guided fractionation to identify active principles for prostate cancer management.

PubMed

Paranjpe, Rutugandha; Gundala, Sushma R; Lakshminarayana, N; Sagwal, Arpana; Asif, Ghazia; Pandey, Anjali; Aneja, Ritu

2013-07-01

Plant extracts, a concoction of bioactive non-nutrient phytochemicals, have long served as the most significant source of new leads for anticancer drug development. Explored for their unique medicinal properties, the leaves of Piper betel, an evergreen perennial vine, are a reservoir of phenolics with antimutagenic, antitumor and antioxidant activities. Here, we show that oral feeding of betel leaf extract (BLE) significantly inhibited the growth of human prostate xenografts implanted in nude mice compared with vehicle-fed controls. To gain insights into the 'active principles', we performed a bioactivity-guided fractionation of methanolic BLE employing solvents of different polarity strengths using classical column chromatography. This approach yielded 15 fractions, which were then pooled to 10 using similar retention factors on thin-layer chromatographs. Bioactivity assays demonstrated that one fraction in particular, F2, displayed a 3-fold better in vitro efficacy to inhibit proliferation of prostate cancer cells than the parent BLE. The presence of phenols, hydroxychavicol (HC) and chavibetol (CHV), was confirmed in F2 by nuclear magnetic resonance, high-performance liquid chromatography and mass spectroscopy. Further, the HC containing F2 subfraction was found to be ~8-fold more potent than the F2 subfraction that contained CHV, in human prostate cancer PC-3 cells as evaluated by the 3-(4,5-dimethylthiazole-2-yl)-2,5-diphenyl tetrazolium bromide assay. Removing CHV from F2 remarkably decreased the IC50 of this fraction, indicating that HC is perhaps the major bioactive constituent, which is present to an extent of 26.59% in BLE. These data provide evidence that HC is a potential candidate for prostate cancer management and warrants further preclinical evaluation.

Neutron crosstalk between liquid scintillators

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

Verbeke, J. M.; Prasad, M. K.; Snyderman, N. J.

2015-05-01

We propose a method to quantify the fractions of neutrons scattering between liquid scintillators. Using a spontaneous fission source, this method can be utilized to quickly characterize an array of liquid scintillators in terms of crosstalk. The point model theory due to Feynman is corrected to account for these multiple scatterings. Using spectral information measured by the liquid scintillators, fractions of multiple scattering can be estimated, and mass reconstruction of fissile materials under investigation can be improved. Monte Carlo simulations of mono-energetic neutron sources were performed to estimate neutron crosstalk. A californium source in an array of liquid scintillators wasmore » modeled to illustrate the improvement of the mass reconstruction.« less

Ion chromatographic determination of sulfur in fuels

NASA Technical Reports Server (NTRS)

Mizisin, C. S.; Kuivinen, D. E.; Otterson, D. A.

1978-01-01

The sulfur content of fuels was determined using an ion chromatograph to measure the sulfate produced by a modified Parr bomb oxidation. Standard Reference Materials from the National Bureau of Standards, of approximately 0.2 + or - 0.004% sulfur, were analyzed resulting in a standard deviation no greater than 0.008. The ion chromatographic method can be applied to conventional fuels as well as shale-oil derived fuels. Other acid forming elements, such as fluorine, chlorine and nitrogen could be determined at the same time, provided that these elements have reached a suitable ionic state during the oxidation of the fuel.

Refined separation of combined Fe–Hf from rock matrices for isotope analyses using AG-MP-1M and Ln-Spec chromatographic extraction resins

PubMed Central

Cheng, Ting; Nebel, Oliver; Sossi, Paolo A.; Chen, Fukun

2014-01-01

A combined procedure for separating Fe and Hf from a single rock digestion is presented. In a two-stage chromatographic extraction process, a purified Fe fraction is first quantitatively separated from the rock matrix using AG-MP-1M resin in HCl. Hafnium is subsequently isolated using a modified version of a commonly applied method using Eichrom LN-Spec resin. Our combined method includes:•Purification of Fe from the rock matrix using HCl, ready for mass spectrometric analysis.•Direct loading of the matrix onto the resin that is used for Hf purification.•Collection of a Fe-free Hf fraction. PMID:26150946

A narrow open tubular column for high efficiency liquid chromatographic separation

DOE PAGES

Chen, Huang; Yang, Yu; Qiao, Zhenzhen; ...

2018-01-01

We report a great feature of open tubular liquid chromatography when it is run using an extremely narrow ( e.g. , 2 μm inner diameter) open tubular column: more than 10 million plates per meter can be achieved in less than 10 min and under an elution pressure of ca. 20 bar.

A narrow open tubular column for high efficiency liquid chromatographic separation

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

Chen, Huang; Yang, Yu; Qiao, Zhenzhen

We report a great feature of open tubular liquid chromatography when it is run using an extremely narrow ( e.g. , 2 μm inner diameter) open tubular column: more than 10 million plates per meter can be achieved in less than 10 min and under an elution pressure of ca. 20 bar.

Jet-mixing of initially-stratified liquid-liquid pipe flows: experiments and numerical simulations

NASA Astrophysics Data System (ADS)

Wright, Stuart; Ibarra-Hernandes, Roberto; Xie, Zhihua; Markides, Christos; Matar, Omar

2016-11-01

Low pipeline velocities lead to stratification and so-called 'phase slip' in horizontal liquid-liquid flows due to differences in liquid densities and viscosities. Stratified flows have no suitable single point for sampling, from which average phase properties (e.g. fractions) can be established. Inline mixing, achieved by static mixers or jets in cross-flow (JICF), is often used to overcome liquid-liquid stratification by establishing unstable two-phase dispersions for sampling. Achieving dispersions in liquid-liquid pipeline flows using JICF is the subject of this experimental and modelling work. The experimental facility involves a matched refractive index liquid-liquid-solid system, featuring an ETFE test section, and experimental liquids which are silicone oil and a 51-wt% glycerol solution. The matching then allows the dispersed fluid phase fractions and velocity fields to be established through advanced optical techniques, namely PLIF (for phase) and PTV or PIV (for velocity fields). CFD codes using the volume of a fluid (VOF) method are then used to demonstrate JICF breakup and dispersion in stratified pipeline flows. A number of simple jet configurations are described and their dispersion effectiveness is compared with the experimental results. Funding from Cameron for Ph.D. studentship (SW) gratefully acknowledged.

Activity of Pure Streptovaricins and Fractionated Streptovaricin Complex Against Friend Virus

PubMed Central

Horoszewicz, Julius S.; Rinehart, Kenneth L.; Leong, Susan S.; Carter, William A.

1975-01-01

Chromatographic fractionation of streptovaricin complex yields two stable components enriched (4- to 16-fold) in activity directed against the polycythemic strain of Friend virus; both components apparently contain no streptovaricins. When compared with their unfractionated parent streptovaricin complex, eight individual intact streptovaricins (A through G and J) show at least a 30-fold reduction in antiviral activity. These results further support the conclusion that the diversified biological properties of streptovaricin complex probably reside in different molecular structures. PMID:237470

Evaluation of the Influence of Sulfur-Fumigated Paeoniae Radix Alba on the Quality of Si Wu Tang by Chromatographic and Chemometric Analysis

PubMed Central

Pei, Ke; Duan, Yu; Qiao, Feng-Xian; Tu, Si-Cong; Liu, Xiao; Wang, Xiao-Li; Song, Xiao-Qing; Fan, Kai-Lei; Cai, Bao-Chang

2016-01-01

An accurate and reliable method of high-performance liquid chromatographic fingerprint combining with multi-ingredient determination was developed and validated to evaluate the influence of sulfur-fumigated Paeoniae Radix Alba on the quality and chemical constituents of Si Wu Tang. Multivariate data analysis including hierarchical cluster analysis and principal component analysis, which integrated with high-performance liquid chromatographic fingerprint and multi-ingredient determination, was employed to evaluate Si Wu Tang in a more objective and scientific way. Interestingly, in this paper, a total of 37 and 36 peaks were marked as common peaks in ten batches of Si Wu Tang containing sun-dried Paeoniae Radix Alba and ten batches of Si Wu Tang containing sulfur-fumigated Paeoniae Radix Alba, respectively, which indicated the changed fingerprint profile of Si Wu Tang when containing sulfur-fumigated herb. Furthermore, the results of simultaneous determination for multiple ingredients showed that the contents of albiflorin and paeoniflorin decreased significantly (P < 0.01) and the contents of gallic acid and Z-ligustilide decreased to some extent at the same time when Si Wu Tang contained sulfur-fumigated Paeoniae Radix Alba. Therefore, sulfur-fumigation processing may have great influence on the quality of Chinese herbal prescription. PMID:27034892

Results from the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

NASA Technical Reports Server (NTRS)

Niemann, Hasso; Atreya, S.; Demick-Monelara, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Owen, T.; Raaen, E.; Way, S.

2006-01-01

The Gas Chromatograph Mass Spectrometer was one of six instruments on the Cassini-Huygens Probe mission to Titan. The GCMS measured in situ the chemical composition of the atmosphere during the probe descent and served as the detector for the pyrolization products for the Aerosol Collector Pyrolyser (ACP) experiment to determine the composition of the aerosol particles. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of mlz from 2 to 141. The major constituents of the lower atmosphere were confirmed to be N2 and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3x10(exp -5) and of Ar-36 is 2.8x10(exp -7). The other primordial noble gases were below 10(exp -8) mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3x10(exp -4). Carbon dioxide, ethane, acetylene and cyanogen were detected evaporating from the surface in addition to methane. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the

Results from the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

NASA Technical Reports Server (NTRS)

Niemann, H.; Atreya, S.; Demick-Montelara, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Owen, T.; Raaen, E.; Way, S.

2006-01-01

The Gas Chromatograph Mass Spectrometer was one of six instruments on the Cassini-Huygens Probe mission to Titan. The GCMS measured in situ the chemical composition of the atmosphere during the probe descent and served as the detector for the pyrolization products for the Aerosol Collector Pyrolyser (ACP) experiment to determine the composition of the aerosol particles. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of m/z from 2 to 141. The major constituents of the lower atmosphere were confirmed to be N2 and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3x10(exp -5) and of Ar-36 is 2.8x10(exp -7). The other primordial noble gases were below 10(exp -8) mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3x10(exp -4). Carbon dioxide, methane, acetylene and cyanogen were detected evaporating from the surface in addition to methane. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the

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

NASA Astrophysics Data System (ADS)

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

2016-04-01

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

Hydrocarbon Liquid Production via Catalytic Hydroprocessing of Phenolic Oils Fractionated from Fast Pyrolysis of Red Oak and Corn Stover

DOE PAGES

Elliott, Douglas C.; Wang, Huamin; Rover, Majorie; ...

2015-04-13

Phenolic oils were produced from fast pyrolysis of two different biomass feedstocks, red oak and corn stover and evaluated in hydroprocessing tests for production of liquid hydrocarbon products. The phenolic oils were produced with a bio-oil fractionating process in combination with a simple water wash of the heavy ends from the fractionating process. Phenolic oils derived from the pyrolysis of red oak and corn stover were recovered with yields (wet biomass basis) of 28.7 wt% and 14.9 wt%, respectively, and 54.3% and 58.6% on a carbon basis. Both precious metal catalysts and sulfided base metal catalyst were evaluated for hydrotreatingmore » the phenolic oils, as an extrapolation from whole bio-oil hydrotreatment. They were effective in removing heteroatoms with carbon yields as high as 81% (unadjusted for the 90% carbon balance). There was nearly complete heteroatom removal with residual O of only 0.4% to 5%, while N and S were reduced to less than 0.05%. Use of the precious metal catalysts resulted in more saturated products less completely hydrotreated compared to the sulfided base metal catalyst, which was operated at higher temperature. The liquid product was 42-52% gasoline range molecules and about 43% diesel range molecules. Particulate matter in the phenolic oils complicated operation of the reactors, causing plugging in the fixed-beds especially for the corn stover phenolic oil. This difficulty contrasts with the catalyst bed fouling and plugging, which is typically seen with hydrotreatment of whole bio-oil. This problem was substantially alleviated by filtering the phenolic oils before hydrotreating. More thorough washing of the phenolic oils during their preparation from the heavy ends of bio-oil or on-line filtration of pyrolysis vapors to remove particulate matter before condensation of the bio-oil fractions is recommended.« less

Hydrocarbon Liquid Production via Catalytic Hydroprocessing of Phenolic Oils Fractionated from Fast Pyrolysis of Red Oak and Corn Stover

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

Elliott, Douglas C.; Wang, Huamin; Rover, Majorie

Phenolic oils were produced from fast pyrolysis of two different biomass feedstocks, red oak and corn stover and evaluated in hydroprocessing tests for production of liquid hydrocarbon products. The phenolic oils were produced with a bio-oil fractionating process in combination with a simple water wash of the heavy ends from the fractionating process. Phenolic oils derived from the pyrolysis of red oak and corn stover were recovered with yields (wet biomass basis) of 28.7 wt% and 14.9 wt%, respectively, and 54.3% and 58.6% on a carbon basis. Both precious metal catalysts and sulfided base metal catalyst were evaluated for hydrotreatingmore » the phenolic oils, as an extrapolation from whole bio-oil hydrotreatment. They were effective in removing heteroatoms with carbon yields as high as 81% (unadjusted for the 90% carbon balance). There was nearly complete heteroatom removal with residual O of only 0.4% to 5%, while N and S were reduced to less than 0.05%. Use of the precious metal catalysts resulted in more saturated products less completely hydrotreated compared to the sulfided base metal catalyst, which was operated at higher temperature. The liquid product was 42-52% gasoline range molecules and about 43% diesel range molecules. Particulate matter in the phenolic oils complicated operation of the reactors, causing plugging in the fixed-beds especially for the corn stover phenolic oil. This difficulty contrasts with the catalyst bed fouling and plugging, which is typically seen with hydrotreatment of whole bio-oil. This problem was substantially alleviated by filtering the phenolic oils before hydrotreating. More thorough washing of the phenolic oils during their preparation from the heavy ends of bio-oil or on-line filtration of pyrolysis vapors to remove particulate matter before condensation of the bio-oil fractions is recommended.« less

Determination of phthalate esters in cleaning and personal care products by dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry.

PubMed

Viñas, Pilar; Campillo, Natalia; Pastor-Belda, Marta; Oller, Ainhoa; Hernández-Córdoba, Manuel

2015-01-09

Phthalic acid esters (PEs) were preconcentrated from cleaning products, detergents and cosmetics using ultrasound assisted extraction (UAE) in the presence of acetonitrile, and then submitted to dispersive liquid-liquid microextraction (DLLME). For DLLME, 3mL of acetonitrile extract, 150μL carbon tetrachloride and 10mL aqueous solution were used. The enriched organic phase was evaporated, reconstituted with 25μL acetonitrile and injected into a liquid chromatograph with a mobile phase (acetonitrile:10mM ammonium acetate, pH 4) under gradient elution. Detection was carried out using both diode-array (DAD) and electrospray-ion trap-tandem mass spectrometry (ESI-IT-MS/MS) in the multiple reaction monitoring mode (MRM) of the positive fragment ions. Quantification was carried out using matrix-matched standards. Detection limits were in the range 0.04-0.45ngmL(-1) for the six PEs considered. The recoveries obtained were in the 84-124% range, with RSDs lower than 10%. Thirty three different cleaning products were analyzed. The most frequently found compound was diethyl phthalate. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous determination of azathioprine and 6-mercaptopurine by high-performance liquid chromatography.

PubMed

Van Os, E C; McKinney, J A; Zins, B J; Mays, D C; Schriver, Z H; Sandborn, W J; Lipsky, J J

1996-04-26

A specific, sensitive, single-step solid-phase extraction and reversed-phase high-performance liquid chromatographic method for the simultaneous determination of plasma 6-mercaptopurine and azathioprine concentrations is reported. Following solid-phase extraction, analytes are separated on a C18 column with mobile phase consisting of 0.8% acetonitrile in 1 mM triethylamine, pH 3.2, run on a gradient system. Quantitation limits were 5 ng/ml and 2 ng/ml for azathioprine and 6-mercaptopurine, respectively. Peak heights correlated linearly to known extracted standards for 6-mercaptopurine and azathioprine (r = 0.999) over a range of 2-200 ng/ml. No chromatographic interferences were detected.

A high-pressure liquid chromatographic method for the determination of N-acetyl-p-aminophenol (acetaminophen) in serum or plasma using a direct injection technique.

PubMed

Manno, B R; Manno, J E; Dempsey, C A; Wood, M A

1981-01-01

N-Acetyl-p-aminophenol (acetaminophen) is becoming more prevalent as an intoxicant in accidental or intentional overdose, therefore, a direct injection ultra-micro high-pressure liquid chromatographic (HPLC) method has been developed for its quantitation. The HPLC analysis was performed using a Model 110 Solvent Metering Pump equipped with a Model 110-19 Pressure Filter (Altex Scientific, Berkeley, CA), a Model 7120 Rheodyne Injector (Rheodyne, Berkeley, CA) or a Model U6K Injector (Waters Associates, Milford, MA) a Model 440 Absorbance Detector (Water's Associates), and a Model 3380A Recorder Integrator (Hewlett Packard, Avondale, PA). A commercially prepared muBonapak C18 Column (Water's Associates) was used. Acetaminophen was eluted with a mixture of 0.01 mol/L aqueous sodium acetate, pH 4.0: acetonitrile (93:7) and the absorbance detector was operated wih a 254 nm filter. The method, which requires only 2 microL of serum or plasma for analysis, offers several distinct advantages to the analyst. No pre- or post-column extraction or other manipulation of the specimen is required to obtain a quantitative result. Rapid processing of the specimen is possible because both acetaminophen and the internal standard are eluted in less than 10 minutes. The small sample (2 microL) is ideal for use with pediatric patients.

Development and validation of a high performance liquid chromatographic method for the separation of exo and endo isomers of granatamine (9-methyl-9-azabicyclo[3.3.1]nonan-3-amine); a key intermediate of granisetron.

PubMed

Krishna, S Radha; Babu, P Suresh; Rao, B M; Rao, N Someswara

2009-12-01

A simple and accurate high-performance liquid chromatographic method was developed for the determination of exo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine in endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine, commercially known as grantamine and used as a key intermediate in the preparation of granisetron bulk drug. Chromatographic separation of the exo and endo isomers of 9-methyl-9-azabicyclo[3.3.1]nonan-3-amine was achieved on an Inertsil C8 column using a mobile phase containing 0.3% trifluoroacetic acid. The resolution between the two isomers was found to be more than 4. The limit of detection (LOD) and limit of quantification (LOQ) of exo isomer were 0.8 and 2.5 microg x mL(-1) respectively, for a 10 microL injection volume. The percentage recovery of exo-isomer ranged from 99 to 102% w/w in the endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine sample. The test solution and mobile phase were observed to be stable up to 48 h after preparation. The validated method yielded good results for precision, linearity, accuracy, robustness and ruggedness. The proposed method was found to be suitable and accurate for the quantitative determination of exo-isomer in bulk samples of endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine.

Pesticide extraction from table grapes and plums using ionic liquid based dispersive liquid-liquid microextraction.

PubMed

Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Angel

2009-12-01

Room temperature ionic liquids (RTILs) have been used as extraction solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of eight multi-class pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox, and fenazaquin) in table grapes and plums. The developed method involves the combination of DLLME and high-performance liquid chromatography with diode array detection. Samples were first homogenized and extracted with acetonitrile. After evaporation and reconstitution of the extract in water containing sodium chloride, a quick DLLME procedure that used the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) and methanol was developed. The RTIL dissolved in a very small volume of acetonitrile was directed injected in the chromatographic system. The comparison between the calibration curves obtained from standards and from spiked sample extracts (matrix-matched calibration) showed the existence of a strong matrix effect for most of the analyzed pesticides. A recovery study was also developed with five consecutive extractions of the two types of fruits spiked at three concentration levels. Mean recovery values were in the range of 72-100% for table grapes and 66-105% for plum samples (except for thiophanate-methyl and carbofuran, which were 64-75% and 58-66%, respectively). Limits of detection (LODs) were in the range 0.651-5.44 microg/kg for table grapes and 0.902-6.33 microg/kg for plums, representing LODs below the maximum residue limits (MRLs) established by the European Union in these fruits. The potential of the method was demonstrated by analyzing 12 commercial fruit samples (six of each type).

Identifying the site of spin trapping in proteins by a combination of liquid chromatography, ELISA, and off-line tandem mass spectrometry.

PubMed

Lardinois, Olivier M; Detweiler, Charles D; Tomer, Kenneth B; Mason, Ronald P; Deterding, Leesa J

2008-03-01

An off-line mass spectrometry method that combines immuno-spin trapping and chromatographic procedures has been developed for selective detection of the nitrone spin trap 5,5-dimethyl-1-pyrroline-N-oxide (DMPO) covalently attached to proteins, an attachment which occurs only subsequent to DMPO trapping of free radicals. In this technique, the protein-DMPO nitrone adducts are digested to peptides with proteolytic agents, peptides from the enzymatic digest are separated by HPLC, and enzyme-linked immunosorbent assays (ELISA) using polyclonal anti-DMPO nitrone antiserum are used to detect the eluted HPLC fractions that contain DMPO nitrone adducts. The fractions showing positive ELISA signals are then concentrated and characterized by tandem mass spectrometry (MS/MS). This method, which constitutes the first liquid chromatography-ELISA-mass spectrometry (LC-ELISA-MS)-based strategy for selective identification of DMPO-trapped protein residues in complex peptide mixtures, facilitates location and preparative fractionation of DMPO nitrone adducts for further structural characterization. The strategy is demonstrated for human hemoglobin, horse heart myoglobin, and sperm whale myoglobin, three globin proteins known to form DMPO-trappable protein radicals on treatment with H(2)O(2). The results demonstrate the power of the new experimental strategy to select DMPO-labeled peptides and identify sites of DMPO covalent attachments.

High-performance liquid chromatographic method for the determination of dansyl-polyamines

Treesearch

Subhash C. Minocha; Rakesh Minocha; Cheryl A. Robie

1990-01-01

This paper describes a fast reliable, and a sensitive technique for the separation and quantification of dansylated polyamines by high-performance liquid chromatography. Using a small 33 x 4.6 mm I.D., 3 ?m particle size, C18 reversed-phase cartridge column and a linear gradient of acetonitrile-heptanesulfonate (10 mM, pH 3.4...

Single-laboratory validation of a high-performance liquid chromatographic-diode array detector-fluorescence detector/mass spectrometric method for simultaneous determination of water-soluble vitamins in multivitamin dietary tablets.

PubMed

Chen, Pei; Atkinson, Renata; Wolf, Wayne R

2009-01-01

The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors [diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS)] for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 microm, 250 x 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100% A (0.1% formic acid in water), a linear gradient to 50% A and 50% B (0.1% formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLDIMS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration.

Single-Laboratory Validation of a High-Performance Liquid Chromatographic-Diode Array Detector-Fluorescence Detector/Mass Spectrometric Method for Simultaneous Determination of Water-Soluble Vitamins in Multivitamin Dietary Tablets

PubMed Central

Chen, Pei; Atkinson, Renata; Wolf, Wayne R.

2014-01-01

The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors [diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS)] for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 µm, 250 × 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100% A (0.1% formic acid in water), a linear gradient to 50% A and 50% B (0.1% formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLD/MS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration. PMID:19485230

Dispersive liquid-liquid microextraction and gas chromatography accurate mass spectrometry for extraction and non-targeted profiling of volatile and semi-volatile compounds in grape marc distillates.

PubMed

Fontana, Ariel; Rodríguez, Isaac; Cela, Rafael

2018-04-20

The suitability of dispersive liquid-liquid microextraction (DLLME) and gas chromatography accurate mass spectrometry (GC-MS), based on a time-of-flight (TOF) MS analyzer and using electron ionization (EI), for the characterization of volatile and semi-volatile profiles of grape marc distillates (grappa) are evaluated. DLLME conditions are optimized with a selection of compounds, from different chemical families, present in the distillate spirit. Under final working conditions, 2.5 mL of sample and 0.5 mL of organic solvents are consumed in the sample preparation process. The absolute extraction efficiencies ranged from 30 to 100%, depending on the compound. For the same sample volume, DLLME provided higher responses than solid-phase microextraction (SPME) for most of the model compounds. The GC-EI-TOF-MS records of grappa samples were processed using a data mining non-targeted search algorithm. In this way, chromatographic peaks and accurate EI-MS spectra of sample components were linked. The identities of more than 140 of these components are proposed from comparison of their accurate spectra with those in a low resolution EI-MS database, accurate masses of most intense fragment ions of known structure, and available chromatographic retention index. The use of chromatographic and spectral data, associated to the set of components mined from different grappa samples, for multivariate analysis purposes is also illustrated in the study. Copyright © 2018 Elsevier B.V. All rights reserved.

Analyzing chromatographic data using multilevel modeling.

PubMed

Wiczling, Paweł

2018-06-01

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

Comprehensive comparison of the chemical and structural characterization of landfill leachate and leonardite humic fractions.

PubMed

Tahiri, Abdelghani; Richel, Aurore; Destain, Jacqueline; Druart, Philippe; Thonart, Philippe; Ongena, Marc

2016-03-01

Humic substances (HS) are complex and heterogeneous mixtures of organic compounds that occur everywhere in the environment. They represent most of the dissolved organic matter in soils, sediments (fossil), water, and landfills. The exact structure of HS macromolecules has not yet been determined because of their complexity and heterogeneity. Various descriptions of HS are used depending on specific environments of origin and research interests. In order to improve the understanding of the structure of HS extracted from landfill leachate (LHS) and commercial HS from leonardite (HHS), this study sought to compare the composition and characterization of the structure of LHS and HHS using elemental composition, chromatographic (high-performance liquid chromatography (HPLC)), and spectroscopic techniques (UV-vis, FTIR, NMR, and MALDI-TOF). The results showed that LHS molecules have a lower molecular weight and less aromatic structure than HHS molecules. The characteristics of functional groups of both LHS and HHS, however, were basically similar, but there was some differences in absorbance intensity. There were also less aliphatic and acidic functional groups and more aromatic and polyphenolic compounds in the humic acid (HA) fraction than in the fulvic acid (FA) and other molecules (OM) fractions of both origins. The differences between LHS and HHS might be due to the time course of humification. Combining the results obtained from these analytical techniques cold improve our understanding of the structure of HS of different origins and thus enhance their potential use.

Liquid Chromatographic Determination of Nitroanilines: An Experiment for the Quantitative Analysis Laboratory.

ERIC Educational Resources Information Center

Cantwell, Frederick F.; Brown, David W.

1981-01-01

Describes a three-hour liquid chromatography experiment involving rapid separation of colored compounds in glass columns packed with a nonpolar absorbent. Includes apparatus design, sample preparation, experimental procedures, and advantages for this determination. (SK)

Chemometrics-assisted chromatographic fingerprinting: An illicit methamphetamine case study.

PubMed

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

2017-03-01

The volatile chemical constituents in complex mixtures can be analyzed using gas chromatography with mass spectrometry. This analysis allows the tentative identification of diverse impurities of an illicit methamphetamine sample. The acquired two-dimensional data of liquid-liquid extraction was resolved by multivariate curve resolution alternating curve resolution to elucidate the embedded peaks effectively. This is the first report on the application of a curve resolution approach for chromatogram fingerprinting to identify particularly the embedded impurities of a drug of abuse. Indeed, the strong and broad peak of methamphetamine makes identifying the underlying peaks problematic and even impossible. Mathematical separation instead of conventional chromatographic approaches was performed in a way that trace components embedded in methamphetamine peak were successfully resolved. Comprehensive analysis of the chromatogram, using multivariate curve resolution, resulted in elution profiles and mass spectra for each pure compound. Impurities such as benzaldehyde, benzyl alcohol, benzene, propenyl methyl ketone, benzyl methyl ketone, amphetamine, N-benzyl-2-methylaziridine, phenethylamine, N,N,α-trimethylamine, phenethylamine, N,α,α-trimethylmethamphetamine, N-acetylmethamphetamine, N-formylmethamphetamine, and other chemicals were identified. A route-specific impurity, N-benzyl-2-methylaziridine, indicating a synthesis route based on ephedrine/pseudoephedrine was identified. Moreover, this is the first report on the detection of impurities such as phenethylamine, N,α,α-trimethylamine (a structurally related impurity), and clonitazene (as an adulterant) in an illicit methamphetamine sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Combined use of algorithms for peak picking, peak tracking and retention modelling to optimize the chromatographic conditions for liquid chromatography-mass spectrometry analysis of fluocinolone acetonide and its degradation products.

PubMed

Fredriksson, Mattias J; Petersson, Patrik; Axelsson, Bengt-Olof; Bylund, Dan

2011-10-17

A strategy for rapid optimization of liquid chromatography column temperature and gradient shape is presented. The optimization as such is based on the well established retention and peak width models implemented in software like e.g. DryLab and LC simulator. The novel part of the strategy is a highly automated processing algorithm for detection and tracking of chromatographic peaks in noisy liquid chromatography-mass spectrometry (LC-MS) data. The strategy is presented and visualized by the optimization of the separation of two degradants present in ultraviolet (UV) exposed fluocinolone acetonide. It should be stressed, however, that it can be utilized for LC-MS analysis of any sample and application where several runs are conducted on the same sample. In the application presented, 30 components that were difficult or impossible to detect in the UV data could be automatically detected and tracked in the MS data by using the proposed strategy. The number of correctly tracked components was above 95%. Using the parameters from the reconstructed data sets to the model gave good agreement between predicted and observed retention times at optimal conditions. The area of the smallest tracked component was estimated to 0.08% compared to the main component, a level relevant for the characterization of impurities in the pharmaceutical industry. Copyright © 2011 Elsevier B.V. All rights reserved.

Chromatographic finger print analysis of anti-inflammatory active extract fractions of aerial parts of Tribulus terrestris by HPTLC technique.

PubMed

Mohammed, Mona Salih; Alajmi, Mohamed Fahad; Alam, Perwez; Khalid, Hassan Subki; Mahmoud, Abelkhalig Muddathir; Ahmed, Wadah Jamal

2014-03-01

To develop HPTLC fingerprint profile of anti-inflammatory active extract fractions of Tribulus terrestris (family Zygophyllaceae). The anti-inflammatory activity was tested for the methanol and its fractions (chloroform, ethyl acetate, n-butanol and aqueous) and chloroform extract of Tribulus terrestris (aerial parts) by injecting different groups of rats (6 each) with carrageenan in hind paw and measuring the edema volume before and 1, 2 and 3 h after carrageenan injection. Control group received saline i.p. The extracts treatment was injected i.p. in doses of 200 mg/kg 1 h before carrageenan administration. Indomethacin (30 mg/kg) was used as standard. HPTLC studies were carried out using CAMAG HPTLC system equipped with Linomat IV applicator, TLC scanner 3, Reprostar 3, CAMAG ADC 2 and WIN CATS-4 software for the active fractions of chloroform fraction of methanol extract. The methanol extract showed good antiedematous effect with percentage of inhibition more than 72%, indicating its ability to inhibit the inflammatory mediators. The methanol extract was re-dissolved in 100 mL of distilled water and fractionated with chloroform, ethyl acetate and n-butanol. The four fractions (chloroform, ethyl acetate, n-butanol and aqueous) were subjected to anti-inflammatory activity. Chloroform fraction showed good anti-inflammatory activity at dose of 200 mg/kg. Chloroform fraction was then subjected to normal phase silica gel column chromatography and eluted with petroleum ether-chloroform, chloroform-ethyl acetate mixtures of increasing polarity which produced 15 fractions (F1-F15). Only fractions F1, F2, F4, F5, F7, F9, F11 and F14 were found to be active, hence these were analyzed with HPTLC to develop their finger print profile. These fractions showed different spots with different Rf values. The different chloroform fractions F1, F2, F4, F5, F7, F9, F11 and F14 revealed 4, 7, 7, 8, 9, 7, 7 and 6 major spots, respectively. The results obtained in this experiment

On-line characterization of monoclonal antibody variants by liquid chromatography-mass spectrometry operating in a two-dimensional format.

PubMed

Alvarez, Melissa; Tremintin, Guillaume; Wang, Jennifer; Eng, Marian; Kao, Yung-Hsiang; Jeong, Justin; Ling, Victor T; Borisov, Oleg V

2011-12-01

Recombinant monoclonal antibodies (MAbs) have become one of the most rapidly growing classes of biotherapeutics in the treatment of human disease. MAbs are highly heterogeneous proteins, thereby requiring a battery of analytical technologies for their characterization. However, incompatibility between separation and subsequent detection is often encountered. Here we demonstrate the utility of a generic on-line liquid chromatography-mass spectrometry (LC-MS) method operated in a two-dimensional format toward the rapid characterization of MAb charge and size variants. Using a single chromatographic system capable of running two independent gradients, up to six fractions of interest from an ion exchange (IEC) or size exclusion (SEC) separation can be identified by trapping and desalting the fractions onto a series of reversed phase trap cartridges with subsequent on-line analysis by mass spectrometry. Analysis of poorly resolved and low-level peaks in the IEC or SEC profile was facilitated by preconcentrating fractions on the traps using multiple injections. An on-line disulfide reduction step was successfully incorporated into the workflow, allowing more detailed characterization of modified MAbs by providing chain-specific information. The system is fully automated, thereby enabling high-throughput analysis with minimal sample handling. This technology provides rapid data turnaround time, a much needed feature during product characterization and development of multiple biotherapeutic proteins. Copyright © 2011 Elsevier Inc. All rights reserved.

[Isolation and immunology identification of spermagglutinating antibodies from human serum].

PubMed

Cibulka, J; Ulcova-Gallová, Z; Balvín, M; Bibková, K; Micanová, Z

2009-06-01

Isolation of spermagglutinating antibodies and their assesment. Retrospective study. Special consulting for reptoduction immunology, Department of Obstetrics and Gynecology, Charles University and Faculty Hospital, Plzen. Fractionation of serum samples by liquid exclusion chromatography, examination of full sera and their chromatographic fractions by Friberg teste (Tray Agglutination Test--TAT), indirect antiimmunoglobulin reaction test (i-MAR test) and by supplementar radial immunodiffusiona (RID). Isolation of spermagglutinating fractions of antisperm antibodies positive sera preserved spermagglutinating aktivity and confirmed great spermagglutinating potential of IgM. According to assesment of the presence of IgG and IgG we reported possible states of immunisation: actual immunisation with IgM activity, perpetual stimulation (IgG and IgM) and, finaly, anamnestic titres in IgG. These findings can help us to choose an optimal way of treatment. Excluding gel chromatography is suitable method for serum proteins fractionation, but not their identification--presence of antisperm antibodies does not affect the chromatographic spectrum, nor the RID patterns.

Development and evaluation of a hydrophilic interaction liquid chromatography-MS/MS method to quantify 19 nucleobases and nucleosides in rat plasma.

PubMed

Du, Yan; Li, Yin-Jie; Hu, Xun-Xiu; Deng, Xu; Qian, Zeng-Ting; Li, Zheng; Guo, Meng-Zhe; Tang, Dao-Quan

2017-04-01

As essential endogenous compounds, nucleobases and nucleosides fulfill various functions in living organisms. This study presents the development and validation of a new hydrophilic interaction liquid chromatography tandem mass spectrometry method for simultaneous quantification of 19 nucleobases and nucleosides in rat plasma. For the sample preparation, 15 kinds of protein precipitants were evaluated according to the chromatographic profile and ion response of analytes. The optimization of chromatographic separation was respectively performed using reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography mode; each separation mode included two test columns with different stationary phases. The chromatographic profile and parameters such as half-width (W 1/2 ), capacity factor (K') and tailing factor (f t ) were used to evaluate the separation efficiencies. Furthermore, the adopted composition of two mobile phase systems and the concentrations of the additives in the optimum buffer system were also investigated. The developed method was fully validated and successfully applied quantitatively to determine 19 nucleobases and nucleosides in plasma from normal and diabetic nephropathy (DN) rats. Significant differences between normal and DN rats were found in plasma levels of cytosine, xanthine, thymidine, adenosine, guanosine, inosine and 8-hydroxy-2'-deoxyguanosine. This information may provide a useful reference for the discovery of potential biomarkers of DN. Copyright © 2016 John Wiley & Sons, Ltd.

A high-performance liquid chromatography assay to monitor the new antiepileptic drug lacosamide in patients with epilepsy.

PubMed

Greenaway, Clare; Ratnaraj, Neville; Sander, Josemir W; Patsalos, Philip N

2010-08-01

A simple high-performance liquid chromatographic micromethod is described for the quantitation of the new antiepileptic drug lacosamide in serum of patients. Serum (100 microL) was first precipitated with 10 microL 60% perchloric acid and 10 microL supernatant injected directly into the high-performance liquid chromatograph. Chromatographic separation was achieved by use of a steel cartridge column (125 x 3 mm inside diameter) packed with Hypersil BDS C-18, at 40 degrees C, and with a gradient elution system comprising methanol, formic acid and water. The eluent was monitored at 215 nm by diode array detection and the calibration curve was linear in the range of 10 to 250 micromol/L. Recovery ranged from 99% to 106%. The limit of quantification was 1 micromol/L and the intrabatch and interbatch coefficients of variation were less than 5%. No interference from commonly prescribed antiepileptic drugs (clobazam, clonazepam, carbamazepine, carbamazepine-10,11-epoxide, gabapentin, lamotrigine, levetiracetam, oxcarbazepine, phenobarbital, phenytoin, primidone, pregabalin, valproic acid, and vigabatrin) was observed, so the method can be used to routinely monitor lacosamide in patients on polytherapy antiepileptic drug regimens.

Liquid Chromatographic Analysis of α-Dicarbonyls Using Girard-T Reagent Derivatives.

PubMed

Lawrence, Glen D; Rahmat, Rozaiha; Makahleh, Ahmad; Saad, Bahruddin

2017-11-01

The measurement of α-dicarbonyls and other degradation products of sugars has become important in view of their toxicity. Although there are several methods used for their analysis, most require long reaction times to form UV absorbing or fluorescent derivatives and the nonpolar nature of commonly used derivatives necessitates relatively high concentrations of organic solvents for elution in reverse phase liquid chromatography. The present method describes the use of Girard-T reagent in a simple, one step derivatization of α-dicarbonyls and conjugated aldehydes and analysis using ion-pair reverse phase liquid chromatography. The limit of detection was in the range of 0.06-0.09 μM (4-12 ng/mL) for glyoxal, methylglyoxal, 3-deoxyglucosone and 5-hydroxymethylfurfural with good linear response and reproducibility using UV detection. The hydrazone derivatives were stable for several days in solution. The method was used to study degradation of several sugars and quantification of the target α-dicarbonyls and 5-hydroxymethylfurfural in several soft drinks. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

[Plasma fractionation in the world: current status].

PubMed

Burnouf, T

2007-05-01

From 22 to 25 million liters of plasma are fractionated yearly in about 70 fractionation plants, either private or government-owned, mainly located in industrialized countries, and with a capacity ranging from 50000 to three million liters. In an increasingly global environment, the plasma industry has recently gone through a major consolidation phase that has seen mergers and acquisitions, and has led to the closure of a number of small plants in Europe. Currently, some fifteen countries are involved into contract plasma fractionation programs to ensure a supply of plasma-derived medicinal products. The majority of the plasma for fractionation is obtained by automated plasmapheresis, the remaining (recovered plasma) being prepared from whole blood as a by-product of red cell production. Plasma for fractionation should be produced, and controlled following well established procedures to meet the strict quality requirements set by regulatory authorities and fractionators. The plasma fractionation technology still relies heavily on the cold ethanol fractionation process, but has been improved by the introduction of modern chromatographic purification methods, and efficient viral inactivation and removal treatments, ensuring quality and safety to a large portfolio of fractionated plasma products. The safety of these products with regards to the risk of transmission of variant Creutzfeldt-Jakob disease seems to be provided, based on current scientific data, by extensive removal of the infectious agent during certain fractionation steps. The leading plasma product is now the intravenous immunoglobulin G, which has replaced factor VIII and albumin in this role. The supply of plasma products (most specifically coagulation products and immunoglobulin) at an affordable price and in sufficient quantity remains an issue; the problem is particularly acute in developing countries, as the switch to recombinant factor VIII in rich countries has not solved the supply issue and has

Gas-liquid chromatographic and gas-liquid-mass spectometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

USGS Publications Warehouse

Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.

1981-01-01

A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

[Immuno-affinity chromatographic purification: the study of methods to test citrinin in monascus products by high performance liquid chromatography].

PubMed

Qiu, Wen-qian; Liu, Xiao-xia; Zheng, Kui-cheng; Fu, Wu-sheng

2012-08-01

To establish a method to test citrinin (CIT) in monascus products by immuno-affinity chromatography (IAC)-high performance liquid chromatography (HPLC), and to detect the content of CIT in monascus products in Fujian province. IAC-HPLC was applied to detect the CIT content in monascus products. The conditions to use HPLC were as follows: C(18) reversed-phase chromatographic column, 150.0 mm×4.6mm×3 µm; mobile phase: the volume ratio of acetonitrile and 0.1% phosphoric acid solution at 65:35; isocratic elution; column temperature: 28°C; flow velocity: 0.8 ml/min; fluorescence detector, excitation wavelength (λ(ex)) was 331 nm and emission wavelength (λ(em)) was 500 nm. The standard curved was established by the linear regression of peak area (Y) to CIT content (X, ng/ml). The accuracy and precision of the method would then be verified. And 32 kinds of monascus products were determined and their color values were compared by this method. The standard curve established in this study was Y = 4634.8X-136.42, r = 1.000; whose limits of detection was 20 µg/kg and the limits of qualification was 64 µg/kg. In the range between 200 and 800 µg/kg, the standard recovery rate was 98.9% - 110.0% (n = 3), and the relative standard deviation (RSD) was 0.51% - 1.76%. Out of the 32 samples, CIT was detected from 11 samples of monascus rice, 9 samples of monascus powder and 5 samples of monascus pigments, the content was around 0.212 - 14.500 mg/kg. 4 out of 7 functional monascus samples were detected out CIT, whose content at 0.142 - 0.275 mg/kg. The method to detect CIT in monascus products by IAC-HPLC has been established.

Flavonoid content and antioxidant capacity of spinach genotypes determined by high-performance liquid chromatography/mass spectrometry

USDA-ARS?s Scientific Manuscript database

Flavonoids in different spinach genotypes were separated, identified, and quantified by a high-performance liquid chromatographic method with photodiode array and mass spectrometric detection. The antioxidant capacities of the genotypes were also measured using two antioxidant assays - oxygen radica...

Fast liquid chromatographic-tandem mass spectrometric method using mixed-mode phase chromatography and solid phase extraction for the determination of 12 mono-hydroxylated brominated diphenyl ethers in human serum.

PubMed

Petropoulou, Syrago-Styliani E; Duong, Wendy; Petreas, Myrto; Park, June-Soo

2014-08-22

Hydroxylated polybrominated diphenyl ethers (OH-PBDEs) are formed from the oxidative metabolism of polybrominated diphenyl ethers (PBDEs) in humans, rats and mice, but their quantitation in human blood and other matrices with liquid chromatography-mass spectrometric techniques has been a challenge. In this study, a novel analytical method was developed and validated using only 250 μL of human serum for the quantitation of twelve OH-PBDEs, fully chromatographically separated in a 15 min analytical run. This method includes two novel approaches: an enzymatic hydrolysis procedure and a chromatographic separation using a mixed mode chromatography column. The enzymatic hydrolysis (EH) was found critical for 4'-OH-BDE17, which was not detectable without it. For the sample clean up, a solid phase extraction protocol was developed and validated for the extraction of the 12 congeners from human serum. In addition, for the first time baseline resolution of two components was achieved that correspond to a single peak previously identified as 6'-OH-BDE99. The method was validated for linearity, accuracy, precision, matrix effects, limit of quantification, limit of detection, sample stability and overall efficiency. Recoveries (absolute and relative) ranged from 66 to 130% with relative standard deviations <21% for all analytes. Limit of detection and quantitation ranged from 4 to 90 pg mL(-1) and 6-120 pg mL(-1), respectively, with no carry over effects. This method was applied in ten commercially available human serum samples from the general US population. The mean values of the congeners detected in all samples are 4'-OH-BDE17 (34.2 pg mL(-1)), 4-OH-BDE42 (33.9 pg mL(-1)), 5-OH-BDE47 (17.5 pg mL(-1)) and 4'-OH-BDE49 (12.4 pg mL(-1)). Copyright © 2014 Elsevier B.V. All rights reserved.

High performance liquid chromatographic determination of ambroxol in the presence of different preservatives in pharmaceutical formulations.

PubMed

Koundourellis, J E; Malliou, E T; Broussali, T A

2000-08-15

A high-performance chromatographic method is described for simultaneous determination of ambroxol in the presence of different preservatives in syrups. The method separates ambroxol from methyl- ethyl-, propyl- and butyl paraben and from other multi-component mixtures. The retention behaviour of ambroxol and parabens as a function of both pH and mobile phase composition was investigated. The eluents were monitored with a UV detector at 247 nm. Linear relationships between the amount of pharmaceutical compounds and peak heights were confirmed at the concentrations of 0.74-14.08 microg ml(-1). The high recovery (no extraction of the samples is required) and the low %RSD confirm the suitability of the proposed method for the determination of ambroxol in different pharmaceutical preparations.

Two-dimensional high-performance liquid chromatographic determination of day-night variation of D-alanine in mammals and factors controlling the circadian changes.

PubMed

Karakawa, Sachise; Miyoshi, Yurika; Konno, Ryuichi; Koyanagi, Satoru; Mita, Masashi; Ohdo, Shigehiro; Hamase, Kenji

2013-10-01

D-Alanine (D-Ala) is one of the naturally occurring D-amino acids in mammals, and its amount is known to have characteristic circadian changes. It is a candidate for a novel physiologically active substance and/or a biomarker, and the regulation mechanisms of the intrinsic amounts of D-Ala are expected to be clarified. In the present study, the effects of the possible factors controlling the D-Ala amounts, e.g., diet, D-amino acid oxidase (DAO) and intestinal bacteria, on the day-night changes in the intrinsic D-Ala amounts have been investigated using a highly sensitive and selective two-dimensional high-performance liquid chromatographic system combining a reversed-phase column and an enantioselective column. The circadian rhythm was not changed under fasting conditions. In the mice lacking D-amino acid oxidase activity (ddY/DAO(-) mice), clear day-night changes were still observed, suggesting that the factors controlling the D-Ala rhythm were not their food and DAO activity. On the other hand, in the germ-free mice, quite low amounts of D-Ala were detected compared with those in the control mice, indicating that the main origin of D-Ala in the mice is intestinal bacteria. Because the D-Ala amounts in the digesta containing intestinal bacteria did not show the day-night changes, the controlling factor of the circadian changes of the D-Ala amount was suggested to be the intestinal absorption.

Theoretical and experimental analysis of a multiphase screw pump, handling gas-liquid mixtures with very high gas volume fractions

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

Raebiger, K.; Faculty of Advanced Technology, University of Glamorgan, Pontypridd, Wales; Maksoud, T.M.A.

In the investigation of the pumping behaviour of multiphase screw pumps, handling gas-liquid mixtures with very high gas volume fractions, theoretical and experimental analyses were performed. A new theoretical screw pump model was developed, which calculates the time-dependent conditions inside the several chambers of a screw pump as well as the exchange of mass and energy between these chambers. By means of the performed experimental analysis, the screw pump model was verified, especially at very high gas volume fractions from 90% to 99%. The experiments, which were conducted with the reference fluids water and air, can be divided mainly intomore » the determination of the steady state pumping behaviour on the one hand and into the analysis of selected transient operating conditions on the other hand, whereas the visualisation of the leakage flows through the circumferential gaps was rounded off the experimental analysis. (author)« less

Avoiding Misannotation of In-Source Fragmentation Products as Cellular Metabolites in Liquid Chromatography–Mass Spectrometry-Based Metabolomics

DOE PAGES

Xu, Yi-Fan; Lu, Wenyun; Rabinowitz, Joshua D.

2015-01-15

Liquid chromatography–mass spectrometry (LC-MS) technology allows for rapid quantitation of cellular metabolites, with metabolites identified by mass spectrometry and chromatographic retention time. Recently, with the development of rapid scanning high-resolution high accuracy mass spectrometers and the desire for high throughput screening, minimal or no chromatographic separation has become increasingly popular. Furthermore, when analyzing complex cellular extracts, however, the lack of chromatographic separation could potentially result in misannotation of structurally related metabolites. Here, we show that, even using electrospray ionization, a soft ionization method, in-source fragmentation generates unwanted byproducts of identical mass to common metabolites. For example, nucleotide-triphosphates generate nucleotide-diphosphates, andmore » hexose-phosphates generate triose-phosphates. We also evaluated yeast intracellular metabolite extracts and found more than 20 cases of in-source fragments that mimic common metabolites. Finally and accordingly, chromatographic separation is required for accurate quantitation of many common cellular metabolites.« less

Novel devices for solvent delivery and temperature programming designed for capillary liquid chromatography.

PubMed

Coutinho, Lincoln Figueira Marins; Nazario, Carlos Eduardo Domingues; Monteiro, Alessandra Maffei; Lanças, Fernando Mauro

2014-08-01

Analyses in chromatographic systems able to save mobile and stationary phases without reducing efficiency and resolution are of current interest. These advantages regarding savings have challenged us to develop a system dedicated to miniaturized liquid chromatography. This paper reports on the development of a high-pressure syringe-type pump, an oven able to perform isothermal and temperature programming and a software program to control these chromatographic devices. The experimental results show that the miniaturized system can generate reproducible and accurate temperature and flow rate. The system was applied to the separation of statins and tetracylines and showed excellent performance. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quality by Design approach in the development of hydrophilic interaction liquid chromatographic method for the analysis of iohexol and its impurities.

PubMed

Jovanović, Marko; Rakić, Tijana; Tumpa, Anja; Jančić Stojanović, Biljana

2015-06-10

This study presents the development of hydrophilic interaction liquid chromatographic method for the analysis of iohexol, its endo-isomer and three impurities following Quality by Design (QbD) approach. The main objective of the method was to identify the conditions where adequate separation quality in minimal analysis duration could be achieved within a robust region that guarantees the stability of method performance. The relationship between critical process parameters (acetonitrile content in the mobile phase, pH of the water phase and ammonium acetate concentration in the water phase) and critical quality attributes is created applying design of experiments methodology. The defined mathematical models and Monte Carlo simulation are used to evaluate the risk of uncertainty in models prediction and incertitude in adjusting the process parameters and to identify the design space. The borders of the design space are experimentally verified and confirmed that the quality of the method is preserved in this region. Moreover, Plackett-Burman design is applied for experimental robustness testing and method is fully validated to verify the adequacy of selected optimal conditions: the analytical column ZIC HILIC (100 mm × 4.6 mm, 5 μm particle size); mobile phase consisted of acetonitrile-water phase (72 mM ammonium acetate, pH adjusted to 6.5 with glacial acetic acid) (86.7:13.3) v/v; column temperature 25 °C, mobile phase flow rate 1 mL min(-1), wavelength of detection 254 nm. Copyright © 2015 Elsevier B.V. All rights reserved.

Chromatographic finger print analysis of anti-inflammatory active extract fractions of aerial parts of Tribulus terrestris by HPTLC technique

PubMed Central

Mohammed, Mona Salih; Alajmi, Mohamed Fahad; Alam, Perwez; Khalid, Hassan Subki; Mahmoud, Abelkhalig Muddathir; Ahmed, Wadah Jamal

2014-01-01

Objective To develop HPTLC fingerprint profile of anti-inflammatory active extract fractions of Tribulus terrestris (family Zygophyllaceae). Methods The anti-inflammatory activity was tested for the methanol and its fractions (chloroform, ethyl acetate, n-butanol and aqueous) and chloroform extract of Tribulus terrestris (aerial parts) by injecting different groups of rats (6 each) with carrageenan in hind paw and measuring the edema volume before and 1, 2 and 3 h after carrageenan injection. Control group received saline i.p. The extracts treatment was injected i.p. in doses of 200 mg/kg 1 h before carrageenan administration. Indomethacin (30 mg/kg) was used as standard. HPTLC studies were carried out using CAMAG HPTLC system equipped with Linomat IV applicator, TLC scanner 3, Reprostar 3, CAMAG ADC 2 and WIN CATS-4 software for the active fractions of chloroform fraction of methanol extract. Results The methanol extract showed good antiedematous effect with percentage of inhibition more than 72%, indicating its ability to inhibit the inflammatory mediators. The methanol extract was re-dissolved in 100 mL of distilled water and fractionated with chloroform, ethyl acetate and n-butanol. The four fractions (chloroform, ethyl acetate, n-butanol and aqueous) were subjected to anti-inflammatory activity. Chloroform fraction showed good anti-inflammatory activity at dose of 200 mg/kg. Chloroform fraction was then subjected to normal phase silica gel column chromatography and eluted with petroleum ether-chloroform, chloroform-ethyl acetate mixtures of increasing polarity which produced 15 fractions (F1-F15). Only fractions F1, F2, F4, F5, F7, F9, F11 and F14 were found to be active, hence these were analyzed with HPTLC to develop their finger print profile. These fractions showed different spots with different Rf values. Conclusions The different chloroform fractions F1, F2, F4, F5, F7, F9, F11 and F14 revealed 4, 7, 7, 8, 9, 7, 7 and 6 major spots, respectively. The

New support for high-performance liquid chromatography based on silica coated with alumina particles.

PubMed

Silveira, José Leandro R; Dib, Samia R; Faria, Anizio M

2014-01-01

A new material based on silica coated with alumina nanoparticles was proposed for use as a chromatographic support for reversed-phase high-performance liquid chromatography. Alumina nanoparticles were synthesized by a sol-gel process in reversed micelles composed of sodium bis(2-ethylhexyl)sulfosuccinate, and the support material was formed by the self-assembly of alumina layers on silica spheres. Spectroscopic and (29)Si nuclear magnetic resonance results showed evidence of chemical bonds between the alumina nanoparticles and the silica spheres, while morphological characterizations showed that the aluminized silica maintained the morphological properties of silica desired for chromatographic purposes after alumina incorporation. Stability studies indicated that bare silica showed high dissolution (~83%), while the aluminized silica remained practically unchanged (99%) after passing one liter of the alkaline mobile phase, indicating high stability under alkaline conditions. The C18 bonded aluminized silica phase showed great potential for use in high-performance liquid chromatography to separate basic molecules in the reversed-phase mode.

Liquid chromatographic assay of ceftizoxime in sera of normal and uremic patients.

PubMed Central

McCormick, E M; Echols, R M; Rosano, T G

1984-01-01

The application of high-pressure liquid chromatography assays for cephalosporin serum concentrations is difficult in uremic patients because of interference from nondialyzable substances. We developed a high-pressure liquid chromatography method for determining the serum concentration of ceftizoxime in normal and uremic patients. The method involves protein precipitation with acetonitrile, followed by removal of the acetonitrile with dichloromethane. Separation was accomplished with a reverse-phase (C-18) column and a mobile phase of 13% acetonitrile and 2.8% acetic acid. UV detection at 310 nm was used to monitor the peaks. This assay produced a linear relationship between peak height ratio and ceftizoxime concentration from 1.5 to 100 micrograms/ml. Samples from 30 patients were assayed by this method and by a bioassay, with a good correlation of results (r = 0.9832). The method was applicable equally to normal and uremic serum samples. PMID:6326665

Identification of marker proteins for the adulteration of meat products with soybean proteins by multidimensional liquid chromatography-tandem mass spectrometry.

PubMed

Leitner, Alexander; Castro-Rubio, Florentina; Marina, Maria Luisa; Lindner, Wolfgang

2006-09-01

Soybean proteins are frequently added to processed meat products for economic reasons and to improve their functional properties. Monitoring of the addition of soybean protein to meat products is of high interest due to the existence of regulations forbidding or limiting the amount of soybean proteins that can be added during the processing of meat products. We have used chromatographic prefractionation on the protein level by perfusion liquid chromatography to isolate peaks of interest from extracts of soybean protein isolate (SPI) and of meat products containing SPI. After enzymatic digestion using trypsin, the collected fractions were analyzed by nanoflow liquid chromatography-tandem mass spectrometry. Several variants and subunits of the major seed proteins, glycinin and beta-conglycinin, were identified in SPI, along with two other proteins. In soybean-protein-containing meat samples, different glycinin A subunits could be identified from the peak discriminating between samples with and without soybean proteins added. Among those, glycinin G4 subunit A4 was consistently found in all samples. Consequently, this protein (subunit) can be used as a target for new analytical techniques in the course of identifying the addition of soybean protein to meat products.

Evaluation of comprehensive multidimensional separations using reversed-phase, reversed-phase liquid chromatography/mass spectrometry for shotgun proteomics.

PubMed

Nakamura, Tatsuji; Kuromitsu, Junro; Oda, Yoshiya

2008-03-01

Two-dimensional liquid-chromatographic (LC) separation followed by mass spectrometric (MS) analysis was examined for the identification of peptides in complex mixtures as an alternative to widely used two-dimensional gel electrophoresis followed by MS analysis for use in proteomics. The present method involves the off-line coupling of a narrow-bore, polymer-based, reversed-phase column using an acetonitrile gradient in an alkaline mobile phase in the first dimension with octadecylsilanized silica (ODS)-based nano-LC/MS in the second dimension. After the first separation, successive fractions were acidified and dried off-line, then loaded on the second dimension column. Both columns separate peptides according to hydrophobicity under different pH conditions, but more peptides were identified than with the conventional technique for shotgun proteomics, that is, the combination of a strong cation exchange column with an ODS column, and the system was robust because no salts were included in the mobile phases. The suitability of the method for proteomics measurements was evaluated.

A Quantitative Gas Chromatographic Ethanol Determination.

ERIC Educational Resources Information Center

Leary, James J.

1983-01-01

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

Chemical variation and fractionation of KREEP basalt magmas

NASA Technical Reports Server (NTRS)

Irving, A. J.

1977-01-01

The fact that 53 Apollo 15 igneous KREEP basalts show a range of 100 Mg/(Mg + Fe) from 73 to 35, and that there are systematic variations in K2O and trace element abundances with the Mg/(Mg + Fe) ratio, suggests that the KREEP basalts are a magma series generated by fractional crystallization processes. Experimental and chemical evidence indicate that this magma series results from low-pressure, possibly subvolcanic, fractional crystallization of a magnesian parental liquid (100 Mg/(Mg + Fe) equal to approximately 72) by removal of low-Ca pyroxene and plagioclase, with eventual production of liquids similar in composition to 15405 quartz-monozodiorites. One soil sample, SAO 465-11, corresponds to the postulated parental liquid, which might have been a direct partial melt of troctolitic materials in the deep lunar crust.

Determination of itopride in human plasma by liquid chromatography coupled to tandem mass spectrometric detection: application to a bioequivalence study.

PubMed

Lee, Heon-Woo; Seo, Ji-Hyung; Choi, Seung-Ki; Lee, Kyung-Tae

2007-01-30

A simple method using a one-step liquid-liquid extraction (LLE) with butyl acetate followed by high-performance liquid chromatography (HPLC) with positive ion electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the determination of itopride in human plasma, using sulpiride as an internal standard (IS). Acquisition was performed in multiple reaction monitoring (MRM) mode, by monitoring the transitions: m/z 359.5>166.1 for itopride and m/z 342.3>111.6 for IS, respectively. Analytes were chromatographed on an YMC C18 reverse-phase chromatographic column by isocratic elution with 1 mM ammonium acetate buffer-methanol (20: 80, v/v; pH 4.0 adjusted with acetic acid). Results were linear (r2=0.9999) over the studied range (0.5-1000 ng mL(-1)) with a total analysis time per run of 2 min for LC-MS/MS. The developed method was validated and successfully applied to bioequivalence studies of itopride hydrochloride in healthy male volunteers.

Determination of drug lipophilicity by phosphatidylcholine-modified microemulsion high-performance liquid chromatography.

PubMed

Xuan, Xueyi; Xu, Liyuan; Li, Liangxing; Gao, Chongkai; Li, Ning

2015-07-25

A new biomembrane-mimetic liquid chromatographic method using a C8 stationary phase and phosphatidylcholine-modified (PC-modified) microemulsion mobile phase was used to estimate unionized and ionized drugs lipophilicity expressed as an n-octanol/water partition coefficient (logP and logD). The introduction of PC into sodium dodecyl sulfate (SDS) microemulsion yielded a good correlation between logk and logD (R(2)=0.8). The optimal composition of the PC-modified microemulsion liquid chromatography (PC-modified MELC) mobile phase was 0.2% PC-3.0% SDS-6.0% n-butanol-0.8% ethyl acetate-90.0% water (pH 7.0) for neutral and ionized molecules. The interactions between the analytes and system described by this chromatographic method is more similar to biological membrane than the n-octanol/water partition system. The result in this paper suggests that PC-modified MELC can serve as a possible alternative to the shake-flask method for high-throughput unionized and ionized drugs lipophilicity determination and simulation of biological processes. Copyright © 2015 Elsevier B.V. All rights reserved.

Environmental impact of flood: the study of arsenic speciation in exchangeable fraction of flood deposits of Warta river (Poland) in determination of "finger prints" of the pollutants origin and the ways of the migration.

PubMed

Kozak, Lidia; Skolasińska, Katarzyna; Niedzielski, Przemysław

2012-09-01

The paper presents the application of the hyphenated technique - high-performance liquid chromatography with atomic absorption spectrometry detection with hydride generation (HPLC-HG-AAS) - in the determinations of inorganic forms of arsenic: As(III) and As(V) in the exchangeable fraction of flood deposits. The separation of analytical signals of the determined arsenic forms was obtained using an ion-exchange column in a chromatographic system with the atomic absorption spectrometer as a detector, at the determination limits of 5 ngg(-1) for As(III) and 10 ngg(-1) for As(V). Flood deposits were collected after big flood event in valley of the Warta river which took place in summer 2010. Samples of overbank deposits were taken in Poznań agglomeration and vicinity (NW Poland). The results of determinations of arsenic forms in the exchangeable fraction of flood deposits allowed indication of a hypothetical path of deposits migration transported by a river during flood and environmental threats posed by their deposition by flood. Copyright © 2012 Elsevier Ltd. All rights reserved.

Three-way principal component analysis of the volatile fraction by HS-SPME/GC of aceto balsamico tradizionale of modena.

PubMed

Cocchi, Marina; Durante, Caterina; Grandi, Margherita; Manzini, Daniela; Marchetti, Andrea

2008-01-15

The present research is aimed at monitoring the evolution of the volatile organic compounds of different samples of aceto balsamico tradizionale of modena (ABTM) during ageing. The flavouring compounds, headspace fraction, of the vinegars of four batterie were sampled by solid phase microextraction technique (SPME), and successively analysed by gas chromatography. Obtaining a data set characterized by different sources of variability such as, different producers, samples of different age and chromatographic profile. The gas chromatographic signals were processed by a three-way data analysis method (Tucker3), which allows an easy visualisation of the data by furnishing a distinct set of graphs for each source of variability. The obtained results indicate that the samples can be separated according to their age highlighting the chemical constituents, which play a major role for their differentiation. The present study represents an example of how the application of Tucker3 models, on gas chromatographic signals may help to follow the transformation processes of food products.

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

PubMed

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

2014-09-19

Metal-organic framework (MOF) HKUST-1 nanoparticles have been incorporated into poly(glycidyl methacrylate-co-ethylene dimethacrylate) (HKUST-1-poly(GMA-co-EDMA)) monoliths to afford stationary phases with enhanced chromatographic performance of small molecules in the reversed phase capillary liquid chromatography. The effect of HKUST-1 nanoparticles in the polymerization mixture on the performance of the monolithic column was explored in detail. While the bare poly(GMA-co-EDMA) monolith exhibited poor resolution (Rs<1.0) and low efficiency (800-16,300plates/m), addition of a small amount of HKUST-1 nanoparticles to the polymerization mixture provide high increased resolution (Rs≥1.3) and high efficiency ranged from 16,300 to 44,300plates/m. Chromatographic performance of HKUST-1-poly(GMA-co-EDMA) monolith was demonstrated by separation of various analytes including polycyclic aromatic hydrocarbons, ethylbenzene and styrene, phenols and aromatic acids using a binary polar mobile phase (CH3CN/H2O). The HKUST-1-poly(GMA-co-EDMA) monolith displayed enhanced hydrophobic and π-π interaction characteristics in the reversed phase separation of test analytes compared to the bare poly(GMA-co-EDMA) monolith. The experiment results showed that HKUST-1-poly(GMA-co-EDMA) monoliths are an alternative to enhance the chromatographic separation of small molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

Improved selectivity for high-performance liquid chromatographic determination of clonazepam in plasma of epileptic patients.

PubMed

Le Guellec, C; Gaudet, M L; Breteau, M

1998-11-20

We report a high-performance liquid chromatography method for clonazepam determination in plasma. The use of a synthetic silica-based stationary phase markedly improved clonazepam resolution compared to standard reversed-phase columns. A liquid-liquid extraction was used, associated with reversed-phase chromatography, gradient elution and ultraviolet detection. Accuracy and precision were satisfactory at therapeutic concentrations. Selectivity was studied for benzodiazepines or other antiepileptic drugs, with particular attention to newly marketed drugs i.e., gabapentine and vigabatrin. No interfering substance was evidenced. Under the conditions described, it was possible to quantify clonazepam at nanogram level even when carbamazepine was present at therapeutic concentrations.

Laser-irradiated drug chromatographic analysis and laser injection of drugs to treat staphyloccocal lesions of skin

NASA Astrophysics Data System (ADS)

Zharov, Vladimir P.; Latyshev, Alexei S.; Kovsh, Anna I.; Razumova, Svetlana A.; Masyukova, Svetlana A.; Volnukhin, Vladimir A.

2001-05-01

This article deals with further development of laser drug delivery methods. In order to estimate the effect of laser- drug interactions, we carried out the chromatographic fractionation of dexamethasone, hydrocortisone, and gentamicine, both prior to and after irradiating them by pulsed Er:YAG laser radiation. The laser radiation parameters were as follows: the wavelength, pulse energy, and pulse duration were, respectively, 2.94 micrometers , 0.7 J, and 100 microsecond(s) . The total laser radiation dose administered to a 100 (mu) l sample of these drug preparations amounted to 150 J. A chromatographic analysis revealed that drug samples exposed to Er:YAG laser radiation did not show any change. The results obtained made it possible to employ pulsed Er:YAG laser radiation to perform laser-acoustic injection of the above-mentioned drug preparations to study the treatment of staphylococcal lesions in 30 guinea pigs. The perforated channel depth was measured and the injected drug solution volume was calculated. It was found that laser injection enabled one to introduce therapeutic doses of drugs, and that it expedited the healing of lesions by 3 to 4 days, as compared to the control group that received the topical application of drugs without laser irradiation.

Isolation and identification of phenolic compounds from rum aged in oak barrels by high-speed countercurrent chromatography/high-performance liquid chromatography-diode array detection-electrospray ionization mass spectrometry and screening for antioxidant activity.

PubMed

Regalado, Erik L; Tolle, Sebastian; Pino, Jorge A; Winterhalter, Peter; Menendez, Roberto; Morales, Ana R; Rodríguez, José L

2011-10-14

Beverages, especially wines are well-known to contain a variety of health-beneficial bioactive substances, mainly of phenolic nature which frequently exhibit antioxidant activity. Significant information is available about the separation and identification of polyphenols from some beverages by chromatographic and spectroscopic techniques, but considerably poor is chemical data related to the polyphenolic content in rums. In this paper, a method involving the all-liquid chromatographic technique of high-speed countercurrent chromatography (HSCCC) combined with high-performance liquid chromatography coupled with diode-array detection and electrospray ionization mass spectrometry (HPLC-DAD-ESI-MS(n)) has been successfully applied for separation and identification of phenolic compounds in an aged rum. Besides, the phenolic fraction (PF) was assayed for its antioxidant effects using three different free radical in vitro assays (DPPH·, RO(2)· and spontaneous lipid peroxidation (LPO) on brain homogenates) and on ferric reducing antioxidant power (FRAP). Results showed that PF potently scavenged DPPH and strongly scavenged peroxyl radicals compared to ascorbic acid and butylated hydroxytoluene (BHT); and almost equally inhibited LPO on brain homogenates subjected to spontaneous LPO when compared to quercetin. Moreover, PF also exhibited strong reducing power. This chemical analysis illustrates the rich array of phenols in the aged rum and represents a rapid and suitable method for the isolation and identification of phenolic compounds from mixtures of considerable complexity, achieving high purity and reproducibility with the use of two separation steps. Copyright © 2011 Elsevier B.V. All rights reserved.

Fractionation of free and conjugated steroids for the detection of boldenone metabolites in calf urine with ultra-performance liquid chromatography/tandem mass spectrometry.

PubMed

Van Poucke, Christof; Van Vossel, Evy; Van Peteghem, Carlos

2008-08-01

For over a decade there has been an intensive debate on the possible natural origin of boldenone (androst-1,4-diene-17beta-ol-3-one, 17beta-boldenone) in calf urine and several alternative markers to discriminate between endogenously formed boldenone and exogenously administered boldenone have been suggested. The currently approved method for proving illegal administration of beta-boldenone(ester) is the detection of beta-boldenone conjugates. In the presented method the sulphate, glucuronide and free fractions are separated from each other during cleanup on a SAX column to be able to determine the conjugated status of the boldenone metabolites. The sulphate and glucuronide fractions are submitted to hydrolysis and all three fractions are further cleaned up on a combination of C18/NH2 solid-phase extraction (SPE) columns. Chromatographic separation of the boldenone metabolites was achieved with a Waters Acquity UPLC instrument using a Sapphire C18 (1.7 microm; 2x50 mm) column within 5 min. Detection of the analytes was achieved by electrospray ionisation tandem mass spectrometry. The decision limits of this method, validated according to Commission Decision 2002/657/EC, were 0.08 ng mL(-1) for androsta-1,4-diene-3,17-dione, 0.13 ng mL(-1) for androst-4-ene-3,17-dione, 0.11 ng mL(-1) for 17alpha-boldenone, 0.07 ng mL(-1) for 17beta-boldenone, 0.24 ng mL(-1) for 5beta-androst-1-en-17beta-ol-3-one and 0.58 ng mL(-1) for 6beta-hydroxy-17beta-boldenone. Because of the fractionation approach used in this method there is no need for conjugated reference standards which often are not available. The disadvantage of needing three analytical runs to determine the conjugated status of each of the metabolites was overcome by using fast chromatography. Copyright (c) 2008 John Wiley & Sons, Ltd.

Entanglement in 3D Kitaev spin liquids

NASA Astrophysics Data System (ADS)

Matern, S.; Hermanns, M.

2018-06-01

Quantum spin liquids are highly fascinating quantum liquids in which the spin degrees of freedom fractionalize. An interesting class of spin liquids are the exactly solvable, three-dimensional Kitaev spin liquids. Their fractionalized excitations are Majonara fermions, which may exhibit a variety of topological band structures—ranging from topologically protected Weyl semi-metals over nodal semi-metals to systems with Majorana Fermi surfaces. We study the entanglement spectrum of such Kitaev spin liquids and verify that it is closely related to the topologically protected edge spectrum. Moreover, we find that in some cases the entanglement spectrum contains even more information about the topological features than the surface spectrum, and thus provides a simple and reliable tool to probe the topology of a system.