Determination of spinosad and its metabolites in meat, milk, cream, and eggs by high-performance liquid chromatography with ultraviolet detection

International Nuclear Information System (INIS)

West, S.D.; Turner, L.G.

1998-01-01

Spinosad is a naturally derived insect-control agent for use on cotton and a variety of other crops. A method is described for the determination of spinosad and its major metabolites in beef and poultry meat, milk, cream, and eggs. The method determines residues of the active ingredients (spinosyns A and D) and two metabolites (spinosyn B and N-demethylspinosyn D). For chicken fat, the method has a limit of quantitation (LOQ) of 0.02 micrograms/g and a limit of detection (LOD) of 0.006 micrograms/g. For all other chicken tissues, beef tissues, milk, cream, and eggs, the method has an LOQ of 0.01 micrograms/g and an LOD of 0.003 micrograms/g. The analytes are extracted from the various sample types using appropriate solvents, and the extracts are purified by liquid-liquid partitioning and solid-phase extraction. All four analytes are determined simultaneously in the purified extracts by reversed-phase high-performance liquid chromatography with ultraviolet detection at 250 nm

Develop of analytic method for the determination of vitamin D3 in multivitaminics and minerals using chromatography it liquidates of high efficiency in normal phase with ultraviolet detection

International Nuclear Information System (INIS)

Solis Barrantes, J. A.

1999-01-01

The good chromatography conditions settled down for the determination vitamin D 3 in multivitaminic samples by means of the analytic technique of chromatography it liquidates of high efficiency (HPLC) in normal phase, with ultraviolet detection to 265 nm. The best conditions in the proposed methodology settled down and the variables of analytic acting were validated, for the analytic quantification of vitamin D 3 in International units. The applicability of the methodology was demonstrated in the vitamin determination D 3 in multivitaminis samples in pill form [es

Determination of rifampicin in human plasma by high-performance liquid chromatography coupled with ultraviolet detection after automatized solid-liquid extraction.

Science.gov (United States)

Louveau, B; Fernandez, C; Zahr, N; Sauvageon-Martre, H; Maslanka, P; Faure, P; Mourah, S; Goldwirt, L

2016-12-01

A precise and accurate high-performance liquid chromatography (HPLC) quantification method of rifampicin in human plasma was developed and validated using ultraviolet detection after an automatized solid-phase extraction. The method was validated with respect to selectivity, extraction recovery, linearity, intra- and inter-day precision, accuracy, lower limit of quantification and stability. Chromatographic separation was performed on a Chromolith RP 8 column using a mixture of 0.05 m acetate buffer pH 5.7-acetonitrile (35:65, v/v) as mobile phase. The compounds were detected at a wavelength of 335 nm with a lower limit of quantification of 0.05 mg/L in human plasma. Retention times for rifampicin and 6,7-dimethyl-2,3-di(2-pyridyl) quinoxaline used as internal standard were respectively 3.77 and 4.81 min. This robust and exact method was successfully applied in routine for therapeutic drug monitoring in patients treated with rifampicin. Copyright © 2016 John Wiley & Sons, Ltd.

Separation and Quantitation of Polyamines in Plant Tissue by High Performance Liquid Chromatography of Their Dansyl Derivatives

Science.gov (United States)

Smith, Mary A.; Davies, Peter J.

1985-01-01

High performance liquid chromatography in combination with fluorescence spectrophotometry can be used to separate and quantitate polyamines (putrescine, cadaverine, spermidine, spermine), prepared as their dansyl derivatives, from plant tissue. The procedure gives sensitive and consistent results for polyamine determinations in plant tissue. In a standard mixture, the minimal detection level was less than 1 picomole of polyamines. PMID:16664216

Improved method for the determination of the cortisol production rate using high-performance liquid chromatography and liquid scintillation counting

NARCIS (Netherlands)

van Ingen, H. E.; Endert, E.

1988-01-01

Two new methods for the determination of the cortisol production rate using reversed-phase high-performance liquid chromatography are described. One uses ultraviolet detection at 205 nm, the other on-line post-column derivatization with benzamidine, followed by fluorimetric detection. The specific

Column Liquid Chromatography.

Science.gov (United States)

Majors, Ronald E.; And Others

1984-01-01

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

Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

International Nuclear Information System (INIS)

Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

2014-01-01

The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag + ) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg −1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm

Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

Energy Technology Data Exchange (ETDEWEB)

Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A., E-mail: joseph.caruso@uc.edu; Landero-Figueroa, Julio

2014-10-01

The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag{sup +}) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg{sup −1} detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

Simultaneous determination of phenytoin, carbamazepine, and 10,11-carbamazepine epoxide in human plasma by high-performance liquid chromatography with ultraviolet detection.

Science.gov (United States)

Bhatti, M M; Hanson, G D; Schultz, L

1998-03-01

The Bioanalytical Chemistry Department at the Madison facility of Covance Laboratories, has developed and validated a simple and sensitive method for the simultaneous determination of phenytoin (PHT), carbamazepine (CBZ) and 10,11-carbamazepine epoxide (CBZ-E) in human plasma by high-performance liquid chromatography with 10,11 dihydrocarbamazepine as the internal standard. Acetonitrile was added to plasma samples containing PHT, CBZ and CBZ-E to precipitate the plasma proteins. After centrifugation, the acetonitrile supernatant was transferred to a clean tube and evaporated under N2. The dried sample extract was reconstituted in 0.4 ml of mobile phase and injected for analysis by high-performance liquid chromatography. Separation was achieved on a Spherisorb ODS2 analytical column with a mobile phase of 18:18:70 acetonitrile:methanol:potassium phosphate buffer. Detection was at 210 nm using an ultraviolet detector. The mean retention times of CBZ-E, PHT and CBZ were 5.8, 9.9 and 11.8 min, respectively. Peak height ratios were fit to a least squares linear regression algorithm with a 1/(concentration)2 weighting. The method produces acceptable linearity, precision and accuracy to a minimum concentration of 0.050 micrograms ml-1 in human plasma. It is also simple and convenient, with no observable matrix interferences.

Validation of a liquid chromatography ultraviolet method for determination of herbicide diuron and its metabolites in soil samples

Directory of Open Access Journals (Sweden)

ANA LUCIA S.M. FELICIO

2016-01-01

Full Text Available ABSTRACT Diuron is one of the most widely herbicide used worldwide, which can undergo degradation producing three primary metabolites: 3,4-dichlorophenylurea, 3-(3,4-dichlorophenyl-1-methylurea, and 3,4-dichloroaniline. Since the persistence of diuron and its by-products in ecosystems involves risk of toxicity to environment and human health, a reliable quantitative method for simultaneous monitoring of these compounds is required. Hence, a simple method without preconcentration step was validated for quantitation of diuron and its main metabolites by high performance liquid chromatography with ultraviolet detection. Separation was achieved in less than 11 minutes using a C18 column, mobile phase composed of acetonitrile and water (45:55 v/v at 0.86 mL min-1 and detection at 254 nm. The validated method using solid-liquid extraction followed by an isocratic chromatographic elution proved to be specific, precise and linear (R2 ˃ 0.99, presenting more than 90% of recovery. The method was successfully applied to quantify diuron and their by-products in soil samples collected in a sugarcane cultivation area, focusing on the environmental control.

Indirect ultraviolet detection of alkaline earth metal ions using an imidazolium ionic liquid as an ultraviolet absorption reagent in ion chromatography.

Science.gov (United States)

Liu, Yong-Qiang; Yu, Hong

2017-04-01

A convenient and versatile method was developed for the separation and detection of alkaline earth metal ions by ion chromatography with indirect UV detection. The chromatographic separation of Mg 2+ , Ca 2+ , and Sr 2+ was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid as the mobile phase, in which the imidazolium ionic liquid acted as an UV-absorption reagent. The effects of imidazolium ionic liquids, detection wavelength, acids in the mobile phase, and column temperature on the retention of Mg 2+ , Ca 2+ , and Sr 2+ were investigated. The main factors influencing the separation and detection were the background UV absorption reagent and the concentration of hydrogen ion in ion chromatography with indirect UV detection. The successful separation and detection of Mg 2+ , Ca 2+ , and Sr 2+ within 14 min were achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.06, 0.12, and 0.23 mg/L, respectively. A new separation and detection method of alkaline earth metal ions by ion chromatography with indirect UV detection was developed, and the application range of ionic liquids was expanded. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the determination of ultraviolet filters in water samples.

Science.gov (United States)

Wang, Huazi; Hu, Lu; Liu, Xinya; Yin, Shujun; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang

2017-09-22

In the present study, a simple and rapid sample preparation method designated ultrasound-assisted dispersive liquid-liquid microextraction based on a deep eutectic solvent (DES) followed by high-performance liquid chromatography with ultraviolet (UV) detection (HPLC-UVD) was developed for the extraction and determination of UV filters from water samples. The model analytes were 2,4-dihydroxybenzophenone (BP-1), benzophenone (BP) and 2-hydroxy-4-methoxybenzophenone (BP-3). The hydrophobic DES was prepared by mixing trioctylmethylammonium chloride (TAC) and decanoic acid (DecA). Various influencing factors (selection of the extractant, amount of DES, ultrasound duration, salt addition, sample volume, sample pH, centrifuge rate and duration) on UV filter recovery were systematically investigated. Under optimal conditions, the proposed method provided good recoveries in the range of 90.2-103.5% and relative standard deviations (inter-day and intra-day precision, n=5) below 5.9%. The enrichment factors for the analytes ranged from 67 to 76. The limits of detection varied from 0.15 to 0.30ngmL -1 , depending on the analytes. The linearities were between 0.5 and 500ngmL -1 for BP-1 and BP and between 1 and 500ngmL -1 for BP-3, with coefficients of determination greater than 0.99. Finally, the proposed method was applied to the determination of UV filters in swimming pool and river water samples, and acceptable relative recoveries ranging from 82.1 to 106.5% were obtained. Copyright © 2017. Published by Elsevier B.V.

Ion-exchanger ultraviolet spectrophotometry for uranium(VI)

International Nuclear Information System (INIS)

Waki, H.; Korkisch, J.

1983-01-01

A sensitive method based on solid-phase spectrophotometry has been developed for the microdetermination of uranium(VI) in water samples. Uranium is sorbed on the anion-exchanger QAE-Sephadex from thiocyanate solution and the absorbance of the exchanger is measured at 300 nm. This method is about 30 times more sensitive than solution spectrophotometry. Absorption spectra of various metals in the anion-exchanger phase are presented and their interferences discussed. A procedure for the cation-exchange separation of uranium from accompanying elements before spectral measurement of uranium is proposed. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

1992-02-10

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

Liquid Chromatography in 1982.

Science.gov (United States)

Freeman, David H.

1982-01-01

Reviews trends in liquid chromatography including apparatus, factors affecting efficient separation of a mixture (peak sharpness and speed), simplified problem-solving, adsorption, bonded phase chromatography, ion selectivity, and size exclusion. The current trend is to control chemical selectivity by the liquid phase. (Author/JN)

Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

NARCIS (Netherlands)

Brudin, S.S.; Shellie, R.A.; Haddad, P.R.; Schoenmakers, P.J.

2010-01-01

In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

Diagnosis of Smith-Lemli-Opitz syndrome by ultraviolet spectrophotometry

Directory of Open Access Journals (Sweden)

F.B. Scalco

2003-10-01

Full Text Available Smith-Lemli-Opitz syndrome (SLOS is an autosomal recessive disorder due to an inborn error of cholesterol metabolism, characterized by congenital malformations, dysmorphism of multiple organs, mental retardation and delayed neuropsychomotor development resulting from cholesterol biosynthesis deficiency. A defect in 3ß-hydroxysteroid-delta7-reductase (delta7-sterol-reductase, responsible for the conversion of 7-dehydrocholesterol (7-DHC to cholesterol, causes an increase in 7-DHC and frequently reduces plasma cholesterol levels. The clinical diagnosis of SLOS cannot always be conclusive because of the remarkable variability of clinical expression of the disorder. Thus, confirmation by the measurement of plasma 7-DHC levels is needed. In the present study, we used a simple, fast, and selective method based on ultraviolet spectrophotometry to measure 7-DHC in order to diagnose SLOS. 7-DHC was extracted serially from 200 µl plasma with ethanol and n-hexane and the absorbance at 234 and 282 nm was determined. The method was applied to negative control plasma samples from 23 normal individuals and from 6 cases of suspected SLOS. The method was adequate and reliable and 2 SLOS cases were diagnosed.

Estratégias para aumento de sensibilidade em espectrofotometria UV-VIS Strategies to increase sensitivity in UV-VIS spectrophotometry

Directory of Open Access Journals (Sweden)

Fábio R. P. Rocha

2004-10-01

Full Text Available Spectrophotometry is one of the most widespread analytical techniques due to its simplicity, reliability, and low-cost instrumentation for both direct measurements and coupled to other techniques or processes such as chromatography, electrophoresis and flow analysis. However, the application is often limited by sensitivity. This article describes some advances that greatly improve the performance of spectrophotometric measurements, especially in order to increase sensitivity, including the employment of liquid-core waveguides and solid-phase spectrophotometry.

Ultraviolet spectrophotometry of three LINERs

Science.gov (United States)

Goodrich, R. W.; Keel, W. C.

1986-01-01

Three galaxies known to be LINERs were observed spectroscopically in the ultraviolet in an attempt to detect the presumed nonthermal continuum source thought to be the source of photoionization in the nuclei. NGC 4501 was found to be too faint for study with the IUE spectrographs, while NGC 5005 had an extended ultraviolet light profile. Comparison with the optical light profile of NGC 5005 indicates that the ultraviolet source is distributed spatially in the same manner as the optical starlight, probably indicating that the ultraviolet excess is due to a component of hot stars in the nucleus. These stars contribute detectable absorption features longward of 2500 A; together with optical data, the IUE spectra suggest a burst of star formation about 1 billion yr ago, with a lower rate continuing to produce a few OB stars. In NGC 4579, a point source contributing most of the ultraviolet excess is found that is much different than the optical light distribution. Furthermore, the ultraviolet to X-ray spectral index in NGC 4579 is 1.4, compatible with the UV to X-ray indices found for samples of Seyfert galaxies. This provides compelling evidence for the detection of the photoionizing continuum in NGC 4579 and draws the research fields of normal galaxies and active galactic nuclei closer together. The emission-line spectrum of NGC 4579 is compared with calculations from a photoionization code, CLOUDY, and several shock models. The photoionization code is found to give superior results, adding to the increasing weight of evidence that the LINER phenomenon is essentially a scaled-down version of the Seyfert phenomenon.

Multi-target determination of organic ultraviolet absorbents in organism tissues by ultrasonic assisted extraction and ultra-high performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Peng, Xianzhi; Jin, Jiabin; Wang, Chunwei; Ou, Weihui; Tang, Caiming

2015-03-06

A sensitive and reliable method was developed for multi-target determination of 13 most widely used organic ultraviolet (UV) absorbents (including UV filters and UV stabilizers) in aquatic organism tissues. The organic UV absorbents were extracted using ultrasonic-assisted extraction, purified via gel permeation chromatography coupled with silica gel column chromatography, and determined by ultra-high performance liquid chromatography-tandem mass spectrometry. Recoveries of the UV absorbents from organism tissues mostly ranged from 70% to 120% from fish filet with satisfactory reproducibility. Method quantification limits were 0.003-1.0ngg(-1) dry weight (dw) except for 2-ethylhexyl 4-methoxycinnamate. This method has been applied to analysis of the UV absorbents in wild and farmed aquatic organisms collected from the Pearl River Estuary, South China. 2-Hydroxy-4-methoxybenzophenone and UV-P were frequently detected in both wild and farmed marine organisms at low ngg(-1)dw. 3-(4-Methylbenzylidene)camphor and most of the benzotriazole UV stabilizers were also frequently detected in maricultured fish. Octocrylene and 2-ethylhexyl 4-methoxycinnamate were not detected in any sample. This work lays basis for in-depth study about bioaccumulation and biomagnification of the UV absorbents in marine environment. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of Biologically Active Compounds from Calendula officinalis Flowers using Spectrophotometry

Directory of Open Access Journals (Sweden)

Butnariu Monica

2012-04-01

Full Text Available Abstract Background This study aimed to quantify the active biological compounds in C. officinalis flowers. Based on the active principles and biological properties of marigolds flowers reported in the literature, we sought to obtain and characterize the molecular composition of extracts prepared using different solvents. The antioxidant capacities of extracts were assessed by using spectrophotometry to measure both absorbance of the colorimetric free radical scavenger 2,2-diphenyl-1-picrylhydrazyl (DPPH as well as the total antioxidant potential, using the ferric reducing power (FRAP assay. Results Spectrophotometric assays in the ultraviolet-visible (UV-VIS region enabled identification and characterization of the full range of phenolic and flavonoids acids, and high-performance liquid chromatography (HPLC was used to identify and quantify phenolic compounds (depending on the method of extraction. Methanol ensured more efficient extraction of flavonoids than the other solvents tested. Antioxidant activity in methanolic extracts was correlated with the polyphenol content. Conclusions The UV-VIS spectra of assimilator pigments (e.g. chlorophylls, polyphenols and flavonoids extracted from the C. officinalis flowers consisted in quantitative evaluation of compounds which absorb to wavelengths broader than 360 nm.

Determination of Five Chemical Markers in DF Formula, the Herbal Composition of Ephedra intermedia, Rheum palmatum, and Lithospermum erythrorhizon, Using High-performance Liquid Chromatography-ultraviolet Detection

Science.gov (United States)

Jeong, Birang; Roh, Jong Seong; Yoon, Michung; Yoon, Yoosik; Shin, Soon Shik; Cho, Hyun Joo; Kwon, Yong Soo; Yang, Heejung

2018-01-01

Background: DF formula is a herbal preparation comprised three medicinal herbs, namely, Ephedra intermedia, Rheum palmatum, and Lithospermum erythrorhizon, which is being used for the treatment of obesity and liver fibrosis in Korean local clinics. Objective: Since the abovementioned three herbs exist with different proportions in DF formula and their chemical markers have different physiochemical properties; it is quite challenging to develop an analytical methodology for the determination of these chemical markers. Materials and Methods: For the analysis of the three herbs, five chemicals, (+)-pseudoephedrine (1) and (−)-ephedrine (2) for E. intermedia, aloe-emodin (3), and chrysophanol (4) for R. palmatum, and shikonin (5) for L. erythrorhizon, were selected for method validation of DF formula, and the analytical conditions were optimized and validated using high-performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). Results: The specificities for the five compounds 1–5 were determined by their UV absorption spectra (1–4: 215 nm and 5: 520 nm). Their calibration curves showed good linear regressions with high correlation coefficient values (R2 > 0.9997). The limits of detection of these five markers were in the range 0.4–2.1 ng/mL, with the exception of 5 (12.7 ng/mL). The intraday variability for all the chemical markers was less than a Relative standard deviation (RSD) of 3%, except for 5 (RSD = 12.6%). In the case of interday analysis, 1 (1.0%), 2 (3.1%), and 4 (3.7%) showed much lower variabilities (RSD High-performance liquid chromatography; UV: Ultraviolet; LOD: Limit of detection; LOQ: Limit of quantification; RSD: Relative standard deviation. PMID:29720825

Pseudo-absolute quantitative analysis using gas chromatography – Vacuum ultraviolet spectroscopy – A tutorial

Energy Technology Data Exchange (ETDEWEB)

Bai, Ling [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); Smuts, Jonathan; Walsh, Phillip [VUV Analytics, Inc., Cedar Park, TX (United States); Qiu, Changling [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); McNair, Harold M. [Department of Chemistry, Virginia Tech, Blacksburg, VA (United States); Schug, Kevin A., E-mail: kschug@uta.edu [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States)

2017-02-08

The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120–240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method. - Highlights: • Gas chromatography diagnostics and quantification using VUV detector. • Absorption cross-sections for molecules enable pseudo-absolute quantitation. • Injection diagnostics reveal systematic errors in hardware settings. • Internal

Pseudo-absolute quantitative analysis using gas chromatography – Vacuum ultraviolet spectroscopy – A tutorial

International Nuclear Information System (INIS)

Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Qiu, Changling; McNair, Harold M.; Schug, Kevin A.

2017-01-01

The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120–240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method. - Highlights: • Gas chromatography diagnostics and quantification using VUV detector. • Absorption cross-sections for molecules enable pseudo-absolute quantitation. • Injection diagnostics reveal systematic errors in hardware settings. • Internal

Simultaneous determination of sulphaquinoxaline and amprolium in veterinary mixture by HPLC and first derivative ultraviolet spectrophotometry

International Nuclear Information System (INIS)

El-Sattar, Osama Abd

2002-01-01

Two simple and reliable methods are described for the determination of sulphaquinoxaline (SQX) and amprolium (AMP) combined in veterinary powder. The first method depends on high performance liquid chromatography on a reversed phase column (Bondapak-C18) using mobile phase consisting of acetonitrile-methanol-water-phosphoric acid (30: 5: 55: 0.7, by volumes) at a flow rate of 1 ml min with UV detection at 254 nm. The detection limits were 0.2 ug ml and 0.35 ug ml and linearity ranges were 2-20 ug ml and 4-40ug ml for SQX and AMP, respectively. The second one deals with the first derivative (D) spectrophotometry with zero-crossing measurement at 253 nm and 226 nm for SQX and AMP respectively. The detection limits were 0.3 ug ml and linearity ranges were 1-18 ug ml and 4-32 ug-ml for SQX and AMP respectively. The proposed procedures were successfully applied to the determination of these drugs in laboratory prepared mixtures with mean percentage recovery ranged from 98.50 to 99.75 and in commercial preparation ranged from 103.85 to 104.85. (author)

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

Science.gov (United States)

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

1978-01-01

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

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

Science.gov (United States)

Çabuk, Hasan; Köktürk, Mustafa

2013-01-01

A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

Directory of Open Access Journals (Sweden)

Hasan Çabuk

2013-01-01

Full Text Available A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

Separation of enantiomers of new psychoactive substances by high-performance liquid chromatography.

Science.gov (United States)

Kadkhodaei, Kian; Forcher, Lisa; Schmid, Martin G

2018-03-01

New psychoactive substances are defined as compounds with consciousness-changing effects and have been developed simultaneously with classical drugs. They arise through structural modifications of illegal substances and are mainly produced to circumvent laws. Availability is simple, since new psychoactive substances can be purchased from the Internet. Among them many chemical drug compound classes are chiral and thus the two resulting enantiomers can differ in their effects. The aim of this study is to develop a suitable chiral high-performance liquid chromatography separation method for a broad spectrum of new psychoactive substances using cellulose tris(3,5-dichlorophenylcarbamate) as a chiral selector. Experiments were performed by high-performance liquid chromatography in normal-phase mode under isocratic conditions using ultraviolet detection. Direct separation was carried out on a high-performance liquid chromatography column (Lux® i-Cellulose-5, 3.5 μm, Phenomenex®), available since 2016. Excellent separation results were obtained for cathinones. After further optimization, even 47 instead of 39 out of 52 cathinones showed baseline separation. For amphetamine derivatives, satisfactory results were not achieved. Further, new psychoactive substances from other compound classes such as benzofuranes, thiophenes, phenidines, phenidates, morpholines, and ketamines were partially resolved, depending on the polarity and degree of substitution. All analytes, which were mainly purchased from the Internet, were proven to be traded as racemates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimizing separations in online comprehensive two‐dimensional liquid chromatography

Science.gov (United States)

Gargano, Andrea F.G.; Schoenmakers, Peter J.

2017-01-01

Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high‐molecular‐weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one‐dimensional liquid chromatography, two‐dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two‐dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two‐dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two‐dimensional liquid chromatography separations. PMID:29027363

High-performance liquid chromatography assay using ultraviolet detection for urinary quantification of milrinone concentrations in cardiac surgery patients undergoing cardiopulmonary bypass.

Science.gov (United States)

Gavra, Paul; Nguyen, Anne Q N; Beauregard, Natasha; Denault, André Y; Varin, France

2014-08-01

An analytical assay using liquid-liquid extraction and high-performance liquid chromatography with ultraviolet detection was developed for the quantification of total (conjugated and unconjugated) urinary concentrations of milrinone after the inhalation of a 5 mg dose in 15 cardiac patients undergoing cardiopulmonary bypass. Urine samples (700 μL) were extracted with ethyl-acetate and subsequently underwent acid back-extraction before and after deconjugation by mild acid hydrolysis. Milrinone was separated on a strong cation exchange analytical column. The mobile phase consisted of a constant mixture of acetonitrile:tetrahydrofurane-NaH2 PO4 buffer (40:60 v/v, pH 3.0). Thirteen calibration curves were linear in the concentration range of 31.25-4000 ng/mL, using olprinone as the internal standard (r(2) range 0.9911-0.9999, n = 13). Mean milrinone recovery and accuracy were respectively 85.2 ± 3.1% and ≥93%. Intra- and inter-day precisions (coefficients of variation) were ≤5% and ≤8%, respectively. Over a 24 h collection period, the cumulative urinary milrinone recovered from 15 patients was 26.1 ± 7.7% of the nominal 5 mg dose administered. The relative amount of milrinone glucuronic acid conjugate was negligible in the urine of patients undergoing cardiopulmonary bypass This method proved to be reliable, specific and accurate to determine the cumulative amount of total milrinone recovered in urine after inhalation. Copyright © 2014 John Wiley & Sons, Ltd.

Optimizing separations in online comprehensive two-dimensional liquid chromatography.

Science.gov (United States)

Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

2018-01-01

Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

Optimizing separations in online comprehensive two‐dimensional liquid chromatography

OpenAIRE

Pirok, Bob W.J.; Gargano, Andrea F.G.; Schoenmakers, Peter J.

2017-01-01

Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass...

Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography.

Science.gov (United States)

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida.

Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography

Science.gov (United States)

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

Objective: In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. Materials and Methods: In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. Results: HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. Conclusion: The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. SUMMARY Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida PMID:26941534

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

International Nuclear Information System (INIS)

Valverde Chavarria, J. C.

1997-01-01

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

Simultaneous determination of polysaccharides and 21 nucleosides and amino acids in different tissues of Salvia miltiorrhiza from different areas by UV-visible spectrophotometry and UHPLC with triple quadrupole MS/MS.

Science.gov (United States)

Xiang, Xiang; Sha, Xiuxiu; Su, Shulan; Zhu, Zhenhua; Guo, Sheng; Yan, Hui; Qian, Dawei; Duan, Jin-Ao

2018-03-01

Salvia miltiorrhiza, a traditional Chinese medicine, is a widely used herbal medicine to treat cardiovascular and cerebrovascular diseases. In this study, ultraviolet (UV)-visible spectrophotometry and ultra-high performance liquid chromatography with triple quadrupole tandem mass spectrometry analytical methods were used for rapid quantification of polysaccharides and 21 nucleosides and amino acids in S. miltiorrhiza to determine 17 samples of different tissues from different areas. Based on the total contents, hierarchical clustering analysis and principal components analysis were performed to classify these samples. The established methods were validated with good linearity, precision, repeatability, stability, and recovery. Chemical analysis revealed a higher content of total analytes in the sample of inflorescence from Nanjing (34.17 mg/g), sample of root and rhizome from Shaanxi (34.13 mg/g) and sample of stem and leaf from Nanjing (31.14 mg/g), respectively, indicating that root and rhizome from Shaanxi and the aerial parts from Nanjing exhibited the highest quality due to their highest content. In addition, contents of nucleosides and amino acids in the aerial parts (14.67 mg/g) were much higher than that in roots and rhizomes (9.17 mg/g). This study suggested that UV-visible spectrophotometry and ultra-high performance liquid chromatography with triple quadrupole tandem mass spectrometry are effective techniques to analyze polysaccharides, nucleosides, and amino acids in plants, and they provided valuable information for the development and utilization value of the aerial parts of S. miltiorrhiza. This analysis would also provide useful information for the quality control of S. miltiorrhiza. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid determination of triclosan in personal care products using new in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction coupled with high performance liquid chromatography-ultraviolet detection.

Science.gov (United States)

Chen, Ming-Jen; Liu, Ya-Ting; Lin, Chiao-Wen; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2013-03-12

This paper describes the development of a novel, simple and efficient in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction (IT-USA-SI-LLME) technique for the rapid determination of triclosan (TCS) in personal care products by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. IT-USA-SI-LLME method is based on the rapid phase separation of water-miscible organic solvent from the aqueous phase in the presence of high concentration of salt (salting-out phenomena) under ultrasonication. In the present work, an indigenously fabricated home-made glass extraction device (8-mL glass tube inbuilt with a self-scaled capillary tip) was utilized as the phase separation device for USA-SI-LLME. After the extraction, the upper extractant layer was narrowed into the self-scaled capillary tip by pushing the plunger plug; thus, the collection and measurement of the upper organic solvent layer was simple and convenient. The effects of various parameters on the extraction efficiency were thoroughly evaluated and optimized. Under optimal conditions, detection was linear in the concentration range of 0.4-100ngmL(-1) with correlation coefficient of 0.9968. The limit of detection was 0.09ngmL(-1) and the relative standard deviations ranged between 0.8 and 5.3% (n=5). The applicability of the developed method was demonstrated for the analysis of TCS in different commercial personal care products and the relative recoveries ranged from 90.4 to 98.5%. The present method was proven to be a simple, sensitive, less organic solvent consuming, inexpensive and rapid procedure for analysis of TCS in a variety of commercially available personal care products or cosmetic preparations. Copyright © 2013 Elsevier B.V. All rights reserved.

Ionic liquid stationary phases for gas chromatography.

Science.gov (United States)

Poole, Colin F; Poole, Salwa K

2011-04-01

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

Certification of caffeine reference material purity by ultraviolet/visible spectrophotometry and high-performance liquid chromatography with diode-array detection as two independent analytical methods.

Science.gov (United States)

Shehata, A B; Rizk, M S; Rend, E A

2016-10-01

Caffeine reference material certified for purity is produced worldwide, but no research work on the details of the certification process has been published in the literature. In this paper, we report the scientific details of the preparation and certification of pure caffeine reference materials. Caffeine was prepared by extraction from roasted and ground coffee by dichloromethane after heating in deionized water mixed with magnesium oxide. The extract was purified, dried, and bottled in dark glass vials. Stratified random selection was applied to select a number of vials for homogeneity and stability studies, which revealed that the prepared reference material is homogeneous and sufficiently stable. Quantification of caffeine purity % was carried out using a calibrated UV/visible spectrophotometer and a calibrated high-performance liquid chromatography with diode-array detection method. The results obtained from both methods were combined to drive the certified value and its associated uncertainty. The certified value of the reference material purity was found to be 99.86% and its associated uncertainty was ±0.65%, which makes the candidate reference material a very useful calibrant in food and drug chemical analysis. Copyright © 2016. Published by Elsevier B.V.

Certification of caffeine reference material purity by ultraviolet/visible spectrophotometry and high-performance liquid chromatography with diode-array detection as two independent analytical methods

Directory of Open Access Journals (Sweden)

A.B. Shehata

2016-10-01

Full Text Available Caffeine reference material certified for purity is produced worldwide, but no research work on the details of the certification process has been published in the literature. In this paper, we report the scientific details of the preparation and certification of pure caffeine reference materials. Caffeine was prepared by extraction from roasted and ground coffee by dichloromethane after heating in deionized water mixed with magnesium oxide. The extract was purified, dried, and bottled in dark glass vials. Stratified random selection was applied to select a number of vials for homogeneity and stability studies, which revealed that the prepared reference material is homogeneous and sufficiently stable. Quantification of caffeine purity % was carried out using a calibrated UV/visible spectrophotometer and a calibrated high-performance liquid chromatography with diode-array detection method. The results obtained from both methods were combined to drive the certified value and its associated uncertainty. The certified value of the reference material purity was found to be 99.86% and its associated uncertainty was ±0.65%, which makes the candidate reference material a very useful calibrant in food and drug chemical analysis.

Hydrazine Determination in Sludge Samples by High Performance Liquid Chromatography

Energy Technology Data Exchange (ETDEWEB)

G. Elias; G. A. Park

2006-02-01

A high-performance liquid chromatographic method using ultraviolet (UV) detection was developed to detect and quantify hydrazine in a variety of environmental matrices. The method was developed primarily for sludge samples, but it is also applicable to soil and water samples. The hydrazine in the matrices was derivatized to their hydrazones with benzaldehyde. The derivatized hydrazones were separated using high performance liquid chromatography (HPLC) with a reversed-phase C-18 column in an isocratic mode with methanol-water (95:5, v/v), and detected with UV detection at 313 nm. The detection limit (25 ml) for the new analytical method is 0.0067 mg ml-1of hydrazine. Hydrazine showed low recovery in soil samples because components in soil oxidized hydrazine. Sludge samples that contained relatively high soil content also showed lower recovery. The technique is relatively simple and cost-effective, and is applicable for hydrazine analysis in different environmental matrices.

Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

Science.gov (United States)

Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

2016-07-01

An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Instrument platforms for nano liquid chromatography.

Science.gov (United States)

Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

2015-11-20

The history of liquid chromatography started more than a century ago and miniaturization and automation are two leading trends in this field. Nanocolumn liquid chromatography (nano LC) and largely synonymous capillary liquid chromatography (capillary LC) are the most recent results of this process where miniaturization of column dimensions and sorbent particle size play crucial role. Very interesting results achieved in the research of extremely miniaturized LC columns at the end of the last century lacked distinctive raison d'être and only advances in mass spectrometry brought a real breakthrough. Configuration of nano LC-electrospray ionization mass spectrometry (LC-ESI-MS) has become a basic tool in bioanalytical chemistry, especially in proteomics. This review discusses and summarizes past and current trends in the realization of nano liquid chromatography (nano LC) platforms. Special attention is given to the mobile phase delivery under nanoflow rates (isocratic, gradient) and sample injection to the nanocolumn. Available detection techniques applied in nano LC separations are also briefly discussed. We followed up the key themes from the original scientific reports over gradual improvements up to the contemporary commercial solutions. Copyright © 2015 Elsevier B.V. All rights reserved.

Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

NARCIS (Netherlands)

Coulier, L.; Kaal, E.R.; Hankemeier, Th.

2006-01-01

The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical

Determination of oxyfluorfen herbicide and oxyfluorfen amine residues in garbanzo beans by liquid chromatography.

Science.gov (United States)

Zhou, M; Miles, C J

1991-01-01

Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.

Determination of insoluble soap in agricultural soil and sewage sludge samples by liquid chromatography with ultraviolet detection.

Science.gov (United States)

Cantarero, Samuel; Zafra-Gómez, Alberto; Ballesteros, Oscar; Navalón, Alberto; Vílchez, José L; Crovetto, Guillermo; Verge, Coral; de Ferrer, Juan A

2010-11-01

We have developed a new analytical procedure for determining insoluble Ca and Mg fatty acid salts (soaps) in agricultural soil and sewage sludge samples. The number of analytical methodologies that focus in the determination of insoluble soap salts in different environmental compartments is very limited. In this work, we propose a methodology that involves a sample clean-up step with petroleum ether to remove soluble salts and a conversion of Ca and Mg insoluble salts into soluble potassium salts using tripotassium ethylenediaminetetraacetate salt and potassium carbonate, followed by the extraction of analytes from the samples using microwave-assisted extraction with methanol. An improved esterification procedure using 2,4-dibromoacetophenone before the liquid chromatography with ultraviolet detection analysis also has been developed. The absence of matrix effect was demonstrated with two fatty acid Ca salts that are not commercial and are never detected in natural samples (C₁₃:₀ and C₁₇:₀). Therefore, it was possible to evaluate the matrix effect because both standards have similar environmental behavior (adsorption and precipitation) to commercial soaps (C₁₀:₀) to C₁₈:₀). We also studied the effect of the different variables on the clean-up, the conversion of Ca soap, and the extraction and derivatization procedures. The quantification limits found ranged from 0.4 to 0.8 mg/kg. The proposed method was satisfactorily applied for the development of a study on soap behavior in agricultural soil and sewage sludge samples. © 2010 SETAC.

High Performance Liquid Chromatography Experiments to Undergraduate Laboratories

Science.gov (United States)

Kissinger, Peter T.; And Others

1977-01-01

Reviews the principles of liquid chromatography with electrochemical detection (LCEC), an analytical technique that incorporates the advantages of both liquids chromatography and electrochemistry. Also suggests laboratory experiments using this technique. (MLH)

performance liquid chromatography

African Journals Online (AJOL)

user

2010-11-22

Nov 22, 2010 ... ISSN 1684–5315 © 2010 Academic Journals. Full Length Research Paper. Determination ... Key words: Processed food, high-performance liquid chromatography, acrylamide, health hazard. INTRODUCTION. In the year 2002, the ... potatoes, breakfast cereals etc. It was thus confirmed that acrylamide has ...

Rapid and selective screening of melamine in bovine milk using molecularly imprinted matrix solid-phase dispersion coupled with liquid chromatography-ultraviolet detection.

Science.gov (United States)

Yan, Hongyuan; Cheng, Xiaoling; Sun, Ning; Cai, Tianyu; Wu, Ruijun; Han, Kun

2012-11-01

A simple, convenient and high selective molecularly imprinted matrix solid-phase dispersion (MI-MSPD) using water-compatible cyromazine-imprinted polymer as adsorbent was proposed for the rapid screening of melamine from bovine milk coupled with liquid chromatography-ultraviolet detection. The molecularly imprinted polymers (MIPs) synthesized by cyromazine as dummy template and reformative methanol-water system as reaction medium showed higher affinity and selectivity to melamine, and so they were applied as the specific dispersant of MSPD to extraction of melamine and simultaneously eliminate the effect of template leakage on quantitative analysis. Under the optimized conditions, good linearity was obtained in a range of 0.24-60.0μgg(-1) with the correlation coefficient of 0.9994. The recoveries of melamine at three spiked levels were ranged from 86.0 to 96.2% with the relative standard deviation (RSD)≤4.0%. This proposed MI-MSPD method combined the advantages of MSPD and MIPs, and could be used as an alternative tool for analyzing the residues of melamine in complex milk samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Simultaneous determination three phytosterol compounds, campesterol, stigmasterol and daucosterol in Artemisia apiacea by high performance liquid chromatography-diode array ultraviolet/visible detector

Science.gov (United States)

Lee, Jiwoo; Weon, Jin Bae; Yun, Bo-Ra; Eom, Min Rye; Ma, Choong Je

2015-01-01

Background: Artemisia apiacea is a traditional herbal medicine using treatment of eczema and jaundice in Eastern Asia, including China, Korea, and Japan. Objective: An accurate and sensitive analysis method using high performance liquid chromatography-diode array ultraviolet/visible detector and liquid chromatography–mass spectrometry for the simultaneous determination of three phytosterol compounds, campesterol, stigmasterol and daucosterol in A. apiacea was established. Materials and Methods: The analytes were separated on a Shiseido C18 column (5 μm, 4.6 mm I.D. ×250 mm) with gradient elution of 0.1% trifluoroacetic acid and acetonitrile. The flow rate was 1 mL/min and detection wavelengths were set at 205 and 254 nm. Results: Validation of the method was performed to demonstrate its linearity, precision and accuracy. The calibration curves showed good linearity (R2 > 0.9994). The limits of detection and limits of quantification were within the ranges 0.55–7.07 μg/mL and 1.67–21.44 μg/mL, respectively. And, the relative standard deviations of intra- and inter-day precision were <2.93%. The recoveries were found to be in the range of 90.03–104.91%. Conclusion: The developed method has been successfully applied to the analysis for quality control of campesterol, stigmasterol and daucosterol in A. apiacea. PMID:25829768

Development of a high performance liquid chromatography method ...

African Journals Online (AJOL)

Development of a high performance liquid chromatography method for simultaneous ... Purpose: To develop and validate a new low-cost high performance liquid chromatography (HPLC) method for ..... Several papers have reported the use of ...

Comprehensive two-dimensional liquid chromatography and hyphenated liquid chromatography to study the degradation of poly(bisphenol A)carbonate

NARCIS (Netherlands)

Coulier, L.; Kaal, E.R.; Hankemeier, T.

2005-01-01

Size exclusion chromatography (SEC), gradient polymer elution chromatography (GPEC) and liquid chromatography at critical conditions (LC-CC) have been developed and applied to observe chemical changes in poly(bisphenol A)carbonate (PC) due to hydrolytic degradation. Especially LC-CC appeared to be

Determination of Chromium(III) Picolinate Using High Performance Liquid Chromatography-Ultraviolet Spectrophotometry

International Nuclear Information System (INIS)

Kim, Sung Il; Woo, Dong Jin; Kang, Dae Kyung; Lee, Myung Hee; Woo, Gun Jo; Cha, Ki Won

2003-01-01

Cr-(pic) 3 has been widely used as food additives, drugs, and feed additives. Accordingly, its determination method should be established. In the present paper, we have studied the determination method of chromium(III) picolinate accurately using ESI-MS on-lined with HPLC. Chromium(III) picolinate in feed products was determined successfully. Chromium(III) is very well known as an essential mineral. It is suggested as a cofactor in the maintenance of both normal lipid and carbohydrate metabolism by assisting the action of insulin on a cell membrane. According to the National Research Council, the daily recommended intake of chromium(III) is 50-200 μg. Several organic chromium(III) complexes have been reported to have significantly higher absorption and tissue incorporation activity than inorganic salts such as chromium(III) chloride

Micellar liquid chromatography

International Nuclear Information System (INIS)

Basova, Elena M; Ivanov, Vadim M; Shpigun, Oleg A

1999-01-01

Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

Determination of Five Chemical Markers in DF Formula, the Herbal Composition of Ephedra intermedia, Rheum palmatum, and Lithospermum erythrorhizon, Using High-performance Liquid Chromatography-ultraviolet Detection.

Science.gov (United States)

Jeong, Birang; Roh, Jong Seong; Yoon, Michung; Yoon, Yoosik; Shin, Soon Shik; Cho, Hyun Joo; Kwon, Yong Soo; Yang, Heejung

2018-01-01

DF formula is a herbal preparation comprised three medicinal herbs, namely, Ephedra intermedia , Rheum palmatum , and Lithospermum erythrorhizon , which is being used for the treatment of obesity and liver fibrosis in Korean local clinics. Since the abovementioned three herbs exist with different proportions in DF formula and their chemical markers have different physiochemical properties; it is quite challenging to develop an analytical methodology for the determination of these chemical markers. For the analysis of the three herbs, five chemicals, (+)-pseudoephedrine (1) and (-)-ephedrine (2) for E. intermedia , aloe-emodin (3), and chrysophanol (4) for R. palmatum , and shikonin (5) for L. erythrorhizon , were selected for method validation of DF formula, and the analytical conditions were optimized and validated using high-performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). The specificities for the five compounds 1-5 were determined by their UV absorption spectra (1-4: 215 nm and 5: 520 nm). Their calibration curves showed good linear regressions with high correlation coefficient values ( R 2 > 0.9997). The limits of detection of these five markers were in the range 0.4-2.1 ng/mL, with the exception of 5 (12.7 ng/mL). The intraday variability for all the chemical markers was less than a Relative standard deviation (RSD) of 3%, except for 5 (RSD = 12.6%). In the case of interday analysis, 1 (1.0%), 2 (3.1%), and 4 (3.7%) showed much lower variabilities (RSD chemical markers showed good recoveries with good accuracies in the range of 90%-110%. The developed HPLC-UV method for the determination of the five chemical markers of the components of DF formula was validated. DF formula, the herbal composition of Ephedra intermedia , Rheum palmatum and Lithospermum erythrorhizon Five chemical markers in DF formula were (+)-pseudoephedrine (1) and (-)-ephedrine (2) for E. intermedia , aloe-emodin (3) and chrysopanol (4) for R. palmatum , and

Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry.

Science.gov (United States)

Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E

2015-09-01

An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. Copyright © 2015. Published by Elsevier B.V.

Application of dispersive liquid-liquid microextraction for the preconcentration of eight parabens in real samples and their determination by high-performance liquid chromatography.

Science.gov (United States)

Shen, Xiong; Liang, Jian; Zheng, Luxia; Lv, Qianzhou; Wang, Hong

2017-11-01

A simple and sensitive method for the simultaneous determination of eight parabens in human plasma and urine samples was developed. The samples were preconcentrated using dispersive liquid-liquid microextraction based on the solidification of floating organic drops and determined by high-performance liquid chromatography with ultraviolet detection. The influence of variables affecting the extraction efficiency was investigated and optimized using Placket-Burman design and Box-Behnken design. The optimized values were: 58 μL of 1-decanol (as extraction solvent), 0.65 mL methanol (as disperser solvent), 1.5% w/v NaCl in 5.0 mL of sample solution, pH 10.6, and 4.0 min centrifugation at 4000 rpm. The extract was injected into the high-performance liquid chromatography system for analysis. Under the optimum conditions, the linear ranges for eight parabens in plasma and urine were 1.0-1000 ng/mL, with correlation coefficients above 0.994. The limit of detection was 0.2-0.4 and 0.1-0.4 ng/mL for plasma and urine samples, respectively. Relative recoveries were between 80.3 and 110.7%, while relative standard deviations were less than 5.4%. Finally, the method was applied to analyze the parabens in 98 patients of primary breast cancer. Results showed that parabens existed widely, at least one paraben detected in 96.9% (95/98) of plasma samples and 98.0% (96/98) of urine samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Conventional high-performance liquid chromatography versus derivative spectrophotometry for the determination of 1,3,6-pyrenetrisulfonic acid trisodium salt and 1,3,6,8-pyrenetetrasulfonic acid tetrasodium salt in the color additive D&C Green No. 8 (Pyranine).

Science.gov (United States)

Jitian, Simion; White, Samuel R; Yang, H-H Wendy; Weisz, Adrian

2014-01-10

Specifications in the U.S. Code of Federal Regulations for the color additive D&C Green No. 8 (Colour Index No. 59040) limit the levels of the subsidiary colors 1,3,6-pyrenetrisulfonic acid trisodium salt (P3S) and 1,3,6,8-pyrenetetrasulfonic acid tetrasodium salt (P4S). The present paper describes a comparative study of two possible methods to replace the currently used multi-step TLC/spectrophotometry method of separating and quantifying the minor components P3S and P4S in G8. One of the new approaches uses conventional high-performance liquid chromatography (HPLC) and the other, derivative spectrophotometry. While the derivative spectrophotometric method was shown to be inadequate for the analysis of minor components overwhelmed by components of much higher concentration, the HPLC method was proven highly effective. The closely related, very polar compounds P3S and P4S were separated by the new HPLC method in less than 4 min using a conventional HPLC instrument. P3S and P4S were quantified by using five-point calibration curves with data points that ranged from 0.45 to 7.63% and from 0.13 to 1.82%, by weight, for P3S and P4S, respectively. The HPLC method was applied to the analysis of test portions from 20 batches of D&C Green No. 8 submitted to the U.S. Food and Drug Administration for certification. Published by Elsevier B.V.

UHPLC: The Greening Face of Liquid Chromatography

OpenAIRE

Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

2013-01-01

Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

Introduction to modern liquid chromatography

National Research Council Canada - National Science Library

Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

2010-01-01

"High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

Dibutylphosphoric acid synthesis

International Nuclear Information System (INIS)

Elias, H.; Boumaout, R.; Kellou, N.; Amedjkouh, A.; Hamidi, A.

1995-09-01

This work consists on the synthesis of dibutylphosphoric acis (DBP) by reaction of butanol with phosphorus pentoxid and on its separation by liquid-liquid extraction. It also deals with the characterization of DBP by some physicochemical analysis methods such as : chromatography, pH-metry and infrared and ultraviolet spectrophotometries. this study showed essentialy, that DBP can be formed in an appreciable amount (55%) when the reaction is realised with butanol/pentoxid molar ratio upper than 3 at temperature of 95 C

Liquid chromatography detection unit, system, and method

Science.gov (United States)

Derenzo, Stephen E.; Moses, William W.

2015-10-27

An embodiment of a liquid chromatography detection unit includes a fluid channel and a radiation detector. The radiation detector is operable to image a distribution of a radiolabeled compound as the distribution travels along the fluid channel. An embodiment of a liquid chromatography system includes an injector, a separation column, and a radiation detector. The injector is operable to inject a sample that includes a radiolabeled compound into a solvent stream. The position sensitive radiation detector is operable to image a distribution of the radiolabeled compound as the distribution travels along a fluid channel. An embodiment of a method of liquid chromatography includes injecting a sample that comprises radiolabeled compounds into a solvent. The radiolabeled compounds are then separated. A position sensitive radiation detector is employed to image distributions of the radiolabeled compounds as the radiolabeled compounds travel along a fluid channel.

Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

Science.gov (United States)

Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

2017-05-01

Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2017-01-01

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

High perfomance liquid chromatography in pharmaceutical analyses.

Science.gov (United States)

Nikolin, Branko; Imamović, Belma; Medanhodzić-Vuk, Saira; Sober, Miroslav

2004-05-01

In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatography replaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography (HPLC) analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1) Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or serum contains numerous endogenous

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

OpenAIRE

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

2017-01-01

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 char...

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from a...

Liquid-adsorption chromatography of metal 8-hydroxyquinolinates

International Nuclear Information System (INIS)

Basova, E.M.; Bol'shova, T.A.; Shirshova, T.S.

1988-01-01

Using the method of liquid-adsorption chromatography separation of 8-hydroxyquinolinates of Cu, Fe, Ga, In, Al, Ni is realized. Thin-layer chromatography (TLC) is used to define the optimum conditions of separation and highly efficient liquid column chromatography (HELC) - for chelate separation. Applicaton of the same sorbent is a very important condition of transition from TLC to HELC. Solica gel Partisil, mobile phase: benzene - isopropanol mixture, containing 1 x 10 -3 M of 8-hydroxyquinoline, are the optimal conditions for the studied chelates separation. But In and Ga in TLC move together, and in HELC they are partially separated, therefore, for their separation the column selectivity should be improved by selection of mobile phase

High performance liquid chromatography in pharmaceutical analyses

Directory of Open Access Journals (Sweden)

Branko Nikolin

2004-05-01

Full Text Available In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatographyreplaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography(HPLC analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1 Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or

21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

Synthesis of monodisperse silica microspheres and modification with diazoresin for mixed-mode ultra high performance liquid chromatography separations.

Science.gov (United States)

Cong, Hailin; Yu, Bing; Tian, Chao; Zhang, Shuai; Yuan, Hua

2017-11-01

Monodisperse silica particles with average diameters of 1.9-2.9 μm were synthesized by a modified Stöber method, in which tetraethyl orthosilicate was continuously supplied to the reaction mixture containing KCl electrolyte, water, ethanol, and ammonia. The obtained silica particles were modified by self-assembly with positively charged photosensitive diazoresin on the surface. After treatment with ultraviolet light, the ionic bonding between silica and diazoresin was converted into covalent bonding through a unique photochemistry reaction of diazoresin. Depending on the chemical structure of diazoresin and mobile phase composition, the diazoresin-modified silica stationary phase showed different separation mechanisms, including reversed phase and hydrophilic interactions. Therefore, a variety of baseline separation of benzene analogues and organic acids was achieved by using the diazoresin-modified silica particles as packing materials in ultra high performance liquid chromatography. According to the π-π interactional difference between carbon rings of fullerenes and benzene rings of diazoresin, C 60 and C 70 were also well separated by ultra-high performance liquid chromatography. Because it has a small size, the ∼2.5 μm monodisperse diazoresin-modified silica stationary phase shows ultra-high efficiency compared with the commercial C 18 -silica high-performance liquid chromatography stationary phase with average diameters of ∼5 μm. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

Science.gov (United States)

Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

2015-06-01

A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Free silanols and ionic liquids as their suppressors in liquid chromatography.

Science.gov (United States)

Buszewska-Forajta, Magdalena; Markuszewski, Michał J; Kaliszan, Roman

2018-07-20

In this review, we will firstly discuss the types and the general properties of silica, focusing on the silica support used in chromatography and capillary electrophoresis. Additionally, the characterization of functional groups (silanols and siloxanes) will be considered in terms of activity of the stationary phases. We will then discuss physical chemistry of the stationary phases applied in liquid chromatography and capillary electrophoresis. The use of ionic liquids as a silanols' suppressors will be presented in the next parts of the study, along with the examples of specific applications. The review is completed with conclusions and an outlook for the future developments in the area of analytical applications of ionic liquids. Copyright © 2018 Elsevier B.V. All rights reserved.

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

Science.gov (United States)

Dawson, V.K.

1982-01-01

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

High-performance liquid chromatography of quinoidal imminium compounds derived from triphenylmethanes

Science.gov (United States)

Abidi, S.L.

1983-01-01

A series of eleven p-aminotriphenylmethane dyes have been studied by high-performance liquid chromatography (HPLC). The combined use of HPLC and spectrophotometry permits specific detection of these compounds in the visible range around 600 nm. As the high affinity of the imminium cations for the active sites of the hydrocarbonaceous stationary phase has presented difficulties for reversed-phase HPLC with pure solvents, organic electrolytes were added to the mobile phase to facilitate the elution of the components with improved selectivity, sensitivity (minimum detection limit, 0.1 μg/ml), and peak symmetry. The effects of chromatographic variables on the component retentivity were investigated. Retention times of the dye analytes decreased with increasing concentration of the added ionic reagent and with decreasing number of the hydrophobic alkyl substituents on the nitrogen atom. The influence of pH on the retention parameters appears to parallel that observed previously for cationic quaternary ammonium compounds. Among the acidic reagents employed, naphthalenesulfonic acid yielded the most satisfactory results. The use of binary electrolyte systems invariably improved the chromatographic behavior of the imminium solutes analyzed. Results obtained with two different octadecylsilica columns have been compared.

Theories to support method development in comprehensive two-dimensional liquid chromatography - A review

NARCIS (Netherlands)

Bedani, F.; Schoenmakers, P.J.; Janssen, H.-G.

2012-01-01

On-line comprehensive two-dimensional liquid chromatography techniques promise to resolve samples that current one-dimensional liquid chromatography methods cannot adequately deal with. To make full use of the potential of two-dimensional liquid chromatography, optimization is required. Optimization

Determination of glucosinolates in 19 Chinese medicinal plants with spectrophotometry and high-pressure liquid chromatography.

Science.gov (United States)

Hu, Ye; Liang, Hao; Yuan, Qipeng; Hong, Yuancheng

2010-08-01

Glucosinolates were evaluated in 19 traditional Chinese medicinal plants involved in seven different families: Brassicaceae, Capparaceae, Euphorbiaceae, Phytolaccaceae, Tropaeolaceae, Caricaceae and Rubiaceae. The total glucosinolate contents were determined by spectrophotometry. Results showed that the high contents of total glucosinolates were found in some herbs of Brassicaceae, Capparaceae and Euphorbiaceae families, while low total glucosinolate contents were observed in two Rubiaceae herbs. In addition, eight glucosinolates (glucoraphanin, glucoraphenin, sinalbin, sinigrin, progoitrin, 4-hydroglucobrassicin, glucoiberin and glucoibervirin) in these herbs were measured using HPLC, and the data showed that individual glucosinolates and their contents varied at different degrees among the distinct species. The highest contents of cancer-protective compounds were found in the seeds of Raphanus sativus L. (glucoraphenin), Sinapis alba (sinalbin) and Phyllanthus emblica L. (sinigrin).

Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

Science.gov (United States)

Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

2017-12-29

Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid phase chromatography on microchips

DEFF Research Database (Denmark)

Kutter, Jörg Peter

2012-01-01

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

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

Science.gov (United States)

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).

Determination of parabens using two microextraction methods coupled with capillary liquid chromatography-UV detection.

Science.gov (United States)

Chen, Chen-Wen; Hsu, Wen-Chan; Lu, Ya-Chen; Weng, Jing-Ru; Feng, Chia-Hsien

2018-02-15

Parabens are common preservatives and environmental hormones. As such, possible detrimental health effects could be amplified through their widespread use in foods, cosmetics, and pharmaceutical products. Thus, the determination of parabens in such products is of particular importance. This study explored vortex-assisted dispersive liquid-liquid microextraction techniques based on the solidification of a floating organic drop (VA-DLLME-SFO) and salt-assisted cloud point extraction (SA-CPE) for paraben extraction. Microanalysis was performed using a capillary liquid chromatography-ultraviolet detection system. These techniques were modified successfully to determine four parabens in 19 commercial products. The regression equations of these parabens exhibited good linearity (r 2 =0.998, 0.1-10μg/mL), good precision (RSD<5%) and accuracy (RE<5%), reduced reagent consumption and reaction times (<6min), and excellent sample versatility. VA-DLLME-SFO was also particularly convenient due to the use of a solidified extract. Thus, the VA-DLLME-SFO technique was better suited to the extraction of parabens from complex matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

Science.gov (United States)

Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

Science.gov (United States)

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.

Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

International Nuclear Information System (INIS)

Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

1994-08-01

Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids

Determination of sodium bis(2-ethylhexylsulfosuccinate (AOT surfactant with liquid chromatography: Comparative study of evaporative light scattering detector, ultraviolet detector and conductivity detector

Directory of Open Access Journals (Sweden)

Ho Ryul Ryu

2010-03-01

Full Text Available This work presents comparison of performance of ultraviolet (UV detector, conductivity detector (CD and evaporative light scattering detector (ELSD in terms of quantitative analysis of AOT (sodium bis(2-ethylhexylsulfosuccinate using liquid chromatography. The employed chromatographic condition, including an acetonitrile/water (45:55, v/v isocratic eluent system, is suitable for the three different detectors, and the figures of merits obtained by building up calibration plots are compared. The sensitivities of the detectors are in the order of ELSD ≈ CD >> UV detector. The linear range for quantification of AOT depends on the type of detector: the lower limits are in the order of UV detector (207 ㎍ mL-1 < CD (310 ㎍ mL-1 << ELSD (930 ㎍ mL-1, while the upper limits are 3720 ㎍ mL-1 for all the detectors (the maximum concentration of injected standard solution. The detection limits are 155 ㎍ mL-1 for ELSD, 78 ㎍ mL-1 for UV detector and 13 ㎍ mL-1 for CD, respectively. The figures of merit for each detector could be a guideline in choosing a detector in quantization of AOT. Furthermore, application of the chromatographic method to two commercial products is demonstrated.

Determination of dasatinib in the tablet dosage form by ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis.

Science.gov (United States)

Gonzalez, Aroa Garcia; Taraba, Lukáš; Hraníček, Jakub; Kozlík, Petr; Coufal, Pavel

2017-01-01

Dasatinib is a novel oral prescription drug proposed for treating adult patients with chronic myeloid leukemia. Three analytical methods, namely ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis, were developed, validated, and compared for determination of the drug in the tablet dosage form. The total analysis time of optimized ultra high performance liquid chromatography and capillary zone electrophoresis methods was 2.0 and 2.2 min, respectively. Direct ultraviolet detection with detection wavelength of 322 nm was employed in both cases. The optimized sequential injection analysis method was based on spectrophotometric detection of dasatinib after a simple colorimetric reaction with folin ciocalteau reagent forming a blue-colored complex with an absorbance maximum at 745 nm. The total analysis time was 2.5 min. The ultra high performance liquid chromatography method provided the lowest detection and quantitation limits and the most precise and accurate results. All three newly developed methods were demonstrated to be specific, linear, sensitive, precise, and accurate, providing results satisfactorily meeting the requirements of the pharmaceutical industry, and can be employed for the routine determination of the active pharmaceutical ingredient in the tablet dosage form. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma.

Science.gov (United States)

Carmo, Ana Paula Barbosa do; Borborema, Manoella; Ribeiro, Stephan; De-Oliveira, Ana Cecilia Xavier; Paumgartten, Francisco Jose Roma; Moreira, Davyson de Lima

2017-01-01

Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD) and quantification (LOQ) limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral) PQ diphosphate. By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.

A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma

Directory of Open Access Journals (Sweden)

Ana Paula Barbosa do Carmo

Full Text Available Abstract INTRODUCTION: Primaquine (PQ diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV analysis of PQ in the blood plasma was developed and validated. METHODS: After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80 (45:55 as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD and quantification (LOQ limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral PQ diphosphate. RESULTS: By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. CONCLUSIONS: The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.

Simultaneous determination of several phytohormones in natural coconut juice by hollow fiber-based liquid-liquid-liquid microextraction-high performance liquid chromatography.

Science.gov (United States)

Wu, Yunli; Hu, Bin

2009-11-06

A simple, selective, sensitive and inexpensive method of hollow fiber-based liquid-liquid-liquid microextraction (HF-LLLME) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV) detection was developed for the determination of four acidic phytohormones (salicylic acid (SA), indole-3-acetic acid (IAA), (+/-) abscisic acid (ABA) and (+/-) jasmonic acid (JA)) in natural coconut juice. To the best of our knowledge, this is the first report on the use of liquid phase microextraction (LPME) as a sample pretreatment technique for the simultaneous analysis of several phytohormones. Using phenetole to fill the pores of hollow fiber as the organic phase, 0.1molL(-1) NaOH solution in the lumen of hollow fiber as the acceptor phase and 1molL(-1) HCl as the donor phase, a simultaneous preconcentration of four target phytohormones was realized. The acceptor phase was finally withdrawn into the microsyringe and directly injected into HPLC for the separation and quantification of the target phytohormones. The factors affecting the extraction efficiency of four phytohormones by HF-LLLME were optimized with orthogonal design experiment, and the data was analyzed by Statistical Product and Service Solutions (SPSS) software. Under the optimized conditions, the enrichment factors for SA, IAA, ABA and JA were 243, 215, 52 and 48, with the detection limits (S/N=3) of 4.6, 1.3, 0.9ngmL(-1) and 8.8 microg mL(-1), respectively. The relative standard deviations (RSDs, n=7) were 7.9, 4.9, 6.8% at 50ngmL(-1) level for SA, IAA, ABA and 8.4% at 500 microg mL(-1) for JA, respectively. To evaluate the accuracy of the method, the developed method was applied for the simultaneous analysis of several phytohormones in five natural coconut juice samples, and the recoveries for the spiked samples were in the range of 88.3-119.1%.

Ultraviolet spectra of Mg in liquid helium

International Nuclear Information System (INIS)

Moriwaki, Y.; Morita, N.

1999-01-01

Emission and absorption spectra of Mg atoms implanted in liquid helium have been observed in the ultraviolet region. We have presented a model of exciplex formation of Mg-He 10 and found that this model is more suitable for understanding the dynamics in the 3s3p 1 P→3s 21 S transition than the bubble model. (orig.)

Characterisation of uremic "Middle molecular"fractions by gas chromatography mass spectrometry, isotachophoresis, and liquid chromatography

NARCIS (Netherlands)

Schoots, A.C.; Mikkers, F.E.P.; Claessens, H.A.; Smet, de R.; Landschoot, van N.; Ringoir, S.M.G.

1982-01-01

Uremic ultrafiltrates (and normal serum, for comparison) were fractionated by means of gel filtration. The collected fractions were further investigated by combined analytical techniques: "high- performance" liquid chromatography, gas chromatography, mass spectrometry, and isotachophoresis.

[Detection of the preservative chlorphenesin in cosmetics by high-performance liquid chromatography].

Science.gov (United States)

Ikarashi, Yoshiaki; Miyazawa, Norimasa; Shimamura, Kimio; Sato, Nobuo; Yoshizawa, Ken-ichi; Hayashi, Masahito; Takano, Katsuhiro; Miyamoto, Michiko; Kojima, Takashi; Sakaguchi, Hiroshi; Fujiio, Makiko

2009-01-01

A simple determination method for preservative chlorphenesin in cosmetics was developed. Cosmetic samples were dissolved in methanol. The sample solution was analyzed by high-performance liquid chromatography (HPLC) with ODS column, using water-methanol (55:45) or water-acetonitrile (3:1) adjusted to pH 2.5 with phosphoric acid as the mobile phase. Chlorphenesin was detected with ultraviolet light detection at 280 nm. A linear relation was obtained between the peak areas and the concentrations of chlorphenesin in the range of 1-500 microg/ml. The determination limit of chlorphenesin was 1-2 microg/ml. Recoveries of chlorphenesin spiked in lotion and milky lotion at the levels of 0.03% and 0.3% were 98.8-100.0%. This method was applied for cosmetics including 0.03% and 0.3% of chlorphenesin and their content corresponded with the determined values.

A combination of solid-phase extraction and dispersive solid-phase extraction effectively reduces the matrix interference in liquid chromatography-ultraviolet detection during pyraclostrobin analysis in perilla leaves.

Science.gov (United States)

Farha, Waziha; Rahman, Md Musfiqur; Abd El-Aty, A M; Jung, Da-I; Kabir, Md Humayun; Choi, Jeong-Heui; Kim, Sung-Woo; Im, So Jeong; Lee, Young-Jun; Shin, Ho-Chul; Kwon, Chan-Hyeok; Son, Young-Wook; Lee, Kang-Bong; Shim, Jae-Han

2015-12-01

Perilla leaves contain many interfering substances; thus, it is difficult to protect the analytes during identification and integration. Furthermore, increasing the amount of sample to lower the detection limit worsens the situation. To overcome this problem, we established a new method using a combination of solid-phase extraction and dispersive solid-phase extraction to analyze pyraclostrobin in perilla leaves by liquid chromatography with ultraviolet absorbance detection. The target compound was quantitated by external calibration with a good determination coefficient (R(2) = 0.997). The method was validated (in triplicate) with three fortification levels, and 79.06- 89.10% of the target compound was recovered with a relative standard deviation <4. The limits of detection and quantification were 0.0033 and 0.01 mg/kg, respectively. The method was successfully applied to field samples collected from two different areas at Gwangju and Muan. The decline in the resiudue concentrations was best ascribed to a first-order kinetic model with half-lives of 5.7 and 4.6 days. The variation between the patterns was attributed to humidity. Copyright © 2015 John Wiley & Sons, Ltd.

Gradient High Performance Liquid Chromatography Method ...

African Journals Online (AJOL)

Purpose: To develop a gradient high performance liquid chromatography (HPLC) method for the simultaneous determination of phenylephrine (PHE) and ibuprofen (IBU) in solid ..... nimesulide, phenylephrine. Hydrochloride, chlorpheniramine maleate and caffeine anhydrous in pharmaceutical dosage form. Acta Pol.

Determination of selected azaarenes in water by bonded-phase extraction and liquid chromatography

Science.gov (United States)

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

1986-01-01

A method for the rapid and simple quantitative determination of quinoline, isoquinoline, and five selected three-ring azaarenes in water has been developed. The azaarene fraction is separated from its carbon analogues on n-octadecyl packing material by edition with acidified water/acetonitrile. Concentration as great as 1000-fold is achieved readily. Instrumental analysis involves high-speed liquid chromatography on flexible-walled, wide-bore columns with fluorescence and ultraviolet detection at several wavelengths employing filter photometers in series. Method-validation data is provided as azaarene recovery efficiency from fortified samples. Distilled water, river water, contaminated ground water, and secondary-treatment effluent have been tested. Recoveries at part-per-billion levels are nearly quantitative for the three-ring compounds, but they decrease for quinoline and isoquinoline. ?? 1986 American Chemical Society.

Determination of five antiarrhythmic drugs in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

Science.gov (United States)

Jouyban, Abolghasem; Sorouraddin, Mohammad Hossein; Farajzadeh, Mir Ali; Somi, Mohammad Hossein; Fazeli-Bakhtiyari, Rana

2015-03-01

A fast and sensitive high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection was developed and validated for the simultaneous quantitation of five antiarrhythmic drugs (metoprolol, propranolol, carvedilol, diltiazem, and verapamil) in human plasma samples. It involves dispersive liquid-liquid microextraction (DLLME) of the desired drugs from 660 µL plasma and separation using isocratic elution with UV detection at 200 nm. The complete separation of all analytes was achieved within 7 min. Acetonitrile (as disperser solvent) resulting from the protein precipitation procedure was mixed with 100 µL dichloromethane (as an extraction solvent) and rapidly injected into 5 mL aqueous solution (pH 11.5) containing 1% (w/v), NaCl. After centrifugation, the sedimented phase containing enriched analytes was collected and evaporated to dryness. The residue was re-dissolved in 50 µL de-ionized water (acidified to pH 3) and injected into the HPLC system for analysis. Under the optimal conditions, the enrichment factors and extraction recoveries ranged between 4.4-10.8 and 33-82%, respectively. The suggested method was linear (r(2) ≥0.997) over a dynamic range of 0.02-0.80 µg mL(-1) in plasma. The intra- and inter-days relative standard deviation (RSD%) and relative error (RE%) values of the method were below 20%, which shows good precision and accuracy. Finally, this method was applied to the analysis of real plasma samples obtained from the patients treated with these drugs. Copyright © 2014 Elsevier B.V. All rights reserved.

Protein separations using enhanced-fluidity liquid chromatography.

Science.gov (United States)

Bennett, Raffeal; Olesik, Susan V

2017-11-10

Enhanced-fluidity liquid chromatography (EFLC) methods using methanol/H 2 O/CO 2 and hydrophilic interaction liquid chromatography (HILIC) were explored for the separation of proteins and peptides. EFLC is a separation mode that uses a mobile phase made of conventional solvents combined with liquid carbon dioxide (CO 2 ) in subcritical conditions. The addition of liquid CO 2 enhances diffusivity and decreases viscosity while maintaining mixture polarity, which typically results in reduced time of analysis. TFA additive and elevated temperature were leveraged as key factors in the separation of a 13-analyte intact protein mixture in under 5min. Under these conditions EFLC showed modest improvement in terms of peak asymmetry and analysis time over the competing ACN/H 2 O separation. Protein analytes detected by electrospray ionization - quadrupole time of flight, were shown to be unaffected by the addition of CO 2 in the mobile phase. Herein, the feasibility of separating hydrophilic proteins up to 80kDa (with transferrin) is demonstrated for CO 2 -containing mobile phases. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultraviolet curing of acrylated liquid natural rubber for surface coating application

OpenAIRE

Kannikar Kwanming; Pairote Klinpituksa; Wae-asae Waehamad

2009-01-01

Ultraviolet curable acrylated liquid natural rubber was prepared by grafting of photosensitive molecule onto liquid natural rubber for surface coating application. The liquid natural rubber (LNR) was firstly obtained by degradation of natural rubber latex with hydrogen peroxide and cobalt acetylacetonate at 65oC for 72 hrs. The preparation of acrylated natural rubber was carried out by the reaction of acrylic acid and epoxidized liquid natural rubber (ELNR) prior obtained from LNR with formic...

High-performance liquid chromatography with fluorescence detection for the rapid analysis of pheophytins and pyropheophytins in virgin olive oil.

Science.gov (United States)

Li, Xueqi; Woodman, Michael; Wang, Selina C

2015-08-01

Pheophytins and pyropheophytin are degradation products of chlorophyll pigments, and their ratios can be used as a sensitive indicator of stress during the manufacturing and storage of olive oil. They increase over time depending on the storage condition and if the oil is exposed to heat treatments during the refining process. The traditional analysis method includes solvent- and time-consuming steps of solid-phase extraction followed by analysis by high-performance liquid chromatography with ultraviolet detection. We developed an improved dilute/fluorescence method where multi-step sample preparation was replaced by a simple isopropanol dilution before the high-performance liquid chromatography injection. A quaternary solvent gradient method was used to include a fourth strong solvent wash on a quaternary gradient pump, which avoided the need to premix any solvents and greatly reduced the oil residues on the column from previous analysis. This new method not only reduces analysis cost and time but shows reliability, repeatability, and improved sensitivity, especially important for low-level samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

Directory of Open Access Journals (Sweden)

Joris Meurs

2016-08-01

Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

High-performance liquid chromatography ultraviolet-photodiode array detection method for aflatoxin B1 in cattle feed supplements

Science.gov (United States)

Mochamad, Lazuardi; Hermanto, Bambang

2017-01-01

Aim: The objective of the current study is to determine the concentration of aflatoxin B1 using high-performance liquid chromatography (HPLC) with a photodiode array (PDA) detector. Materials and Methods: Aflatoxin B1 certified reference grade from Trilogy Analytical Laboratory dissolved acetonitrile (ACN) at 10 µg/mL was using standard assessment. HPLC instruments such as ultraviolet-PDA detector used a Shimadzu LC-6AD pump with DGU-20A5 degasser, communication module-20A, and PDA detector SPD-M20A with FRC-10A fraction collector. The HPLC was set isocratic method at 354 nm with a reverse-phase ODS C18 column (LiChrospher® 100 RP-18; diameter, 5 µm) under a 20°C controlled column chamber. Rheodyne® sample loops were performed in 20 µL capacities. The mobile phase was performed at fraction 63:26:11 H2O: methanol:ACN at pH 6.8. A total of 1 kg of feed contained 10% bread crumbs and 30% concentrated, 40% forage, and 20% soybean dregs were using commercials samples. Samples were extracted by ACN and separated with solid phase extraction ODS 1 mL than elution with mobile phase to collect at drying samples performed. The samples were ready to use after added 1 mL mobile phase than injected into the system of HPLC. Results: We found that the retention time of aflatoxin B1 was approximately 10.858 min. Linearity of 0.01-0.08 µg/mL aflatoxin B1 dissolved in mobile phase was obtained at R2=0.9. These results demonstrate that these methods can be used to analyze aflatoxin B1 and gain 89-99% recovery. The limit of detection of this assay was obtained at 3.5 × 10−6 µg/mL. Conclusion: This method was easy to apply and suitable to analyzing at small concentrations of aflatoxin B1 in formulated product of feed cattle. PMID:28919686

On-line high-performance liquid chromatography-ultraviolet-nuclear magnetic resonance method of the markers of nerve agents for verification of the Chemical Weapons Convention.

Science.gov (United States)

Mazumder, Avik; Gupta, Hemendra K; Garg, Prabhat; Jain, Rajeev; Dubey, Devendra K

2009-07-03

This paper details an on-flow liquid chromatography-ultraviolet-nuclear magnetic resonance (LC-UV-NMR) method for the retrospective detection and identification of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the markers of the toxic nerve agents for verification of the Chemical Weapons Convention (CWC). Initially, the LC-UV-NMR parameters were optimized for benzyl derivatives of the APAs and AAPAs. The optimized parameters include stationary phase C(18), mobile phase methanol:water 78:22 (v/v), UV detection at 268nm and (1)H NMR acquisition conditions. The protocol described herein allowed the detection of analytes through acquisition of high quality NMR spectra from the aqueous solution of the APAs and AAPAs with high concentrations of interfering background chemicals which have been removed by preceding sample preparation. The reported standard deviation for the quantification is related to the UV detector which showed relative standard deviations (RSDs) for quantification within +/-1.1%, while lower limit of detection upto 16mug (in mug absolute) for the NMR detector. Finally the developed LC-UV-NMR method was applied to identify the APAs and AAPAs in real water samples, consequent to solid phase extraction and derivatization. The method is fast (total experiment time approximately 2h), sensitive, rugged and efficient.

Determination of Polymer Additives-Antioxidants, Ultraviolet Stabilizers, Plasticizers and Photoinitiators in Plastic Food Package by Accelerated Solvent Extraction Coupled with High-Performance Liquid Chromatography.

Science.gov (United States)

Li, Bo; Wang, Zhi-Wei; Lin, Qin-Bao; Hu, Chang-Ying; Su, Qi-Zhi; Wu, Yu-Mei

2015-07-01

An analytical method for the quantitative determination of 4 antioxidants, 9 ultraviolet (UV) stabilizers, 12 phthalate plasticizers and 2 photoinitiators in plastic food package using accelerated solvent extraction (ASE) coupled with high-performance liquid chromatography-photodiode array detector (HPLC-PDA) has been developed. Parameters affecting the efficiency in the process such as extraction and chromatographic conditions were studied in order to determine operating conditions. The analytical method of ASE-HPLC showed good linearity with good correlation coefficients (R ≥ 0.9833). The limits of detection and quantification were between 0.03 and 0.30 µg mL(-1) and between 0.10 and 1.00 µg mL(-1) for 27 analytes. Average spiked recoveries for most analytes in samples were >70.4% at 10, 20 and 40 µg g(-1) spiked levels, except UV-9 and Irganox 1010 (58.6 and 64.0% spiked at 10 µg g(-1), respectively), the relative standard deviations were in the range from 0.4 to 15.4%. The methodology has been proposed for the analysis of 27 polymer additives in plastic food package. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Radioactivity monitor for high-performance liquid chromatography

International Nuclear Information System (INIS)

Reeve, D.R.; Crozier, A.

1977-01-01

The coupling of a homogeneous radioactivity monitor to a liquid chromatograph involves compromises between the sensitivity of the monitor and the resolution and speed of analysis of the chromatograph. The theoretical relationships between these parameters are considered and expressions derived which make it possible to calculate suitable monitor operating conditions for most types of high-performance liquid chromatography

Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

Science.gov (United States)

Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

2015-12-01

Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of niacin and pyridoxine at trace levels by using diode array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry.

Science.gov (United States)

Sel, Sabriye; Öztürk Er, Elif; Bakırdere, Sezgin

2017-12-01

A highly sensitive and simple diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method was developed for the simultaneous determination of niacin and pyridoxine in pharmaceutical drugs, tap water, and wastewater samples. To determine the in vivo behavior of niacin and pyridoxine, analytes were subjected to simulated gastric conditions. The calibration plots of the diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method showed good linearity over a wide concentration range with close to 1.0 correlation coefficients for both analytes. The limit of detection/limit of quantitation values for liquid chromatography quadrupole time-of-flight tandem mass spectrometry analysis were 1.98/6.59 and 1.3/4.4 μg/L for niacin and pyridoxine, respectively, while limit of detection/limit of quantitation values for niacin and pyridoxine in high-performance liquid chromatography analysis were 3.7/12.3 and 5.7/18.9 μg/L, respectively. Recovery studies were also performed to show the applicability of the developed methods, and percentage recovery values were found to be 90-105% in tap water and 94-97% in wastewater for both analytes. The method was also successfully applied for the qualitative and quantitative determination of niacin and pyridoxine in drug samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent development of ionic liquid stationary phases for liquid chromatography.

Science.gov (United States)

Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

2015-11-13

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

Liquid chromatography in migration studies

International Nuclear Information System (INIS)

Carlsen, L.; Batsberg, W.

1982-01-01

Liquid chromatography ahs been suggested as a facile experimental technique to determine important physico-chemical properties, as permeability, porosity, dispersion-, diffusion-, and sorption charcteristics for geological material as chalk samples. The feasibility of the trechnique as a rapid method to evaluate the possible influence of changes in ground water composition on the migration behavior of radionuclides has been demonstrated

Liquid chromatography-tandem mass spectrometry detection of the quaternary ammonium compound mebezonium as an active ingredient in t61.

Science.gov (United States)

Kirschbaum, Katrin M; Grellner, Wolfgang; Rochholz, Gertrud; Musshoff, Frank; Madea, Burkhard

2011-03-01

Quaternary ammonium compounds pose an analytical challenge. Mebezonium, a muscle-relaxing agent contained in veterinary euthanasia solution T61, was analyzed in body fluids, organs, and injection sites of a veterinarian by liquid chromatography-tandem mass spectrometry (LC-MS-MS) method. Additionally, embutramide and tetracaine, which are two other active ingredients contained in T61, methadone, xylazine, and analgesics were detected by LC-MS-MS and high-performance liquid chromatography-ultraviolet detection methods. For detection of mebezonium a solid-phase extraction (SPE) combined with ionpairing reagent heptafluorobutyric acid was developed. Separation was achieved on Phenomenex Synergi Hydro RP C(18) column combined with ammonium formate buffer and acetonitrile (pH 3.5). To enrich other drugs, liquid-liquid extraction procedures were used. Most of these drugs were separated on a Restek Allure PFP Propyl column using the mentioned mobile phase. Mebezonium and embutramide were detected in femoral vein serum in concentrations of 10.9 and 2.0 mg/L, respectively. The concentration of xylazine and methadone in serum was 2.0 and 0.4 mg/L, respectively. The LC-MS-MS method with SPE combined with an ion-pairing reagent allowed the quantitation of mebezonium. Methadone was detected in toxic concentrations and was, in combination with xylazine and T61, considered to be the cause of death.

Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

Science.gov (United States)

Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

2013-12-15

A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

High-Performance Liquid Chromatography-Mass Spectrometry.

Science.gov (United States)

Vestal, Marvin L.

1984-01-01

Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

Science.gov (United States)

Hemmati, Maryam; Asghari, Alireza; Bazregar, Mohammad; Rajabi, Maryam

2016-11-01

In this research work, an efficient tandem dispersive liquid-liquid microextraction (TDLLME) procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was successfully applied for the determination of beta-blockers in human plasma and pharmaceutical wastewater samples. High clean-up and preconcentration factor are easily and rapidly feasible via this novel, cheap, and safe microextraction method, leading to high quality experimental data. It consists of two sequential dispersive liquid-liquid microextraction methods, accomplished via air/ultrasonic agitation and air agitation, respectively. In order to enrich the optimal values for the mentioned procedures, the Box-Behnken design (BBD) combined with the desirability function (DF) was used. The optimum values were found to be 11.0 % (w/v) of the salt amount, an initial pH value of 12.0, 103 μL of organic extractant phase, and 45 μL of aqueous extractant phase with pH value of 2.0, resulted in reasonable recovery percentages with a logical desirability. Under optimal experimental conditions, good linear ranges (3-2000 ng mL -1 for metoprolol and 2.5-2500 ng mL -1 for propranolol with the correlation of determinations (R 2 s) higher than 0.99) and low limits of detection (0.8 and 1.0 ng mL -1 for propranolol and metoprolol, respectively) were obtainable. Also, TDLLME-HPLC-UV provided good proper repeatabilities (relative standard deviations (RSDs) below 5.7 %, n = 3) and high enrichment factors (EFs) of 75-100. Graphical abstract TDLLME of beta-blockers from complicated matrices.

[Analysis of microalbuminuria with immunonephelometry and high performance liquid chromatography. Evaluation of new criteria].

Science.gov (United States)

Markó, Lajos; Molnár, Gergo Attila; Wagner, Zoltán; Koszegi, Tamás; Matus, Zoltán; Mohás, Márton; Kuzma, Mónika; Szijártó, István András; Wittmann, István

2008-01-13

Hypertension as well as type 2 diabetes mellitus is a major factor in population mortality. Both diseases damage the endothelium, the early sign of which is microalbuminuria, which can be screened by dipstick and can be diagnosed by using immuno-based and high performance liquid chromatography methods. Using high performance liquid chromatography, the non-immunoreactive albumin can be detected as well. The authors aimed at the examination of albuminuria in the case of immunonephelometrically negative patients with high performance liquid chromatography, in diabetic and hypertensive and non-diabetic hypertensive populations. The authors also wanted to compare the present (albumin-creatinine ratio: male: > or =2.5 mg/mmol, female: > or =3.5 mg/mmol) and a new criteria of the Heart Outcomes Prevention Evaluation study (patients without diabetes: immunological method, > or =0.7 mg/mmol; high performance liquid chromatography, > or =3.1 mg/mmol; individuals with diabetes: immunological method, > or =1.4 mg/mmol; high performance liquid chromatography, > or =5.2 mg/mmol) of microalbuminuria. Examination of fresh urines of 469 microalbuminuria negative patients by dipstick were performed by immunonephelometry. Patients, who were microalbuminuria negative by immunonephelometry as well, were further analyzed by high performance liquid chromatography using the Accumintrade mark Kit, based on size-exclusion chromatography. Three times higher albuminuria were found with high performance liquid chromatography than with immunonephelometry. The intraindividual coefficient of variation did not differ in the two methods (37 +/- 31% vs. 40 +/- 31%, p = 0.869; immunonephelometry vs. high performance liquid chromatography; mean +/- standard deviation). Using the present criteria for microalbuminuria, 43% of immunonephelometrically negative patients proved to be microalbuminuric by high performance liquid chromatography. Using the new criteria of the Heart Outcomes Prevention

Microcystin Detection Characteristics of Fluorescence Immunochromatography and High Performance Liquid Chromatography

International Nuclear Information System (INIS)

Pyo, Dong Jin; Park, Geun Young; Choi, Jong Chon; Oh, Chang Suk

2005-01-01

Different detection characteristics of fluorescence immunochromatography method and high performance liquid chromatography (HPLC) method for the analysis of cyanobacterial toxins were studied. In particular, low and high limits of detection, detection time and reproducibility and detectable microcystin species were compared when fluorescence immunochromatography method and high performance liquid chromatography method were applied for the detection of microcystin (MC), a cyclic peptide toxin of the freshwater cyanobacterium Microcystis aeruginosa. A Fluorescence immunochromatography assay system has the unique advantages of short detection time and low detection limit, and high performance liquid chromatography detection method has the strong advantage of individual quantifications of several species of microcystins

Application of ionic liquids in liquid chromatography and electrodriven separation.

Science.gov (United States)

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.

Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

Science.gov (United States)

Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

2017-10-13

A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid-phase microextraction and fibre-optics-based cuvetteless CCD-array micro-spectrophotometry for trace analysis

International Nuclear Information System (INIS)

Sharma, Nisha; Pillai, Aradhana K.K.V.; Pathak, Neeraj; Jain, Archana; Verma, Krishna K.

2009-01-01

Liquid-phase microextraction (LPME) has been investigated for trace analysis in the present work in conjunction with fibre-optic-based micro-spectrophotometry which accommodates sample volume of 1 μL placed between the two ends of optical fibres. Methods have been evolved for the determination of (i) 1-100 μM and 0.5-20 μM of thiols by single drop microextraction (SDME) and LPME in 25 μL of the organic solvent, respectively, involving their reaction with the Ellman reagent and ion pair microextraction of thiolate ion formed; (ii) 70 μg to 7 mg L -1 of chlorine/chlorine dioxide by headspace in-drop reaction with alternative reagents, viz., mixed phenylhydrazine-4-sulphonic acid and N-(1-naphthyl)ethylenediamine dihydrochloride, o-dianisidine, o-tolidine, and N,N-diethyl-p-phenylenediamine; (iii) 0.2-4 mg L -1 of ammonia by reaction with 2,4-dinitro-1-fluorobenzene to give 2,4-dinitroaniline which was diazotized and coupled with 1-naphthylamine, the resulting dye was subjected to preconcentration by solid-phase extraction and LPME; and (iv) 25-750 μg L -1 of iodide/total iodine by oxidation of iodide by 2-iodosobenzoate, microextraction of iodine in organic solvent, and re-extraction into aqueous starch-iodide reagent drop held in the organic phase. LPME using 25-30 μL of organic solvent was found to produce more sensitive results than SDME. The cuvetteless spectrophotometry as used in combination with sample handling techniques produced limits of detection of analytes which were better than obtained by previously reported spectrophotometry.

Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

International Nuclear Information System (INIS)

Mroczek, Tomasz; Ndjoko-Ioset, Karine; Glowniak, Kazimierz; Mietkiewicz-Capala, Agnieszka; Hostettmann, Kurt

2006-01-01

From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C 18 column using a gradient elution. Based on MS n spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide

Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mroczek, Tomasz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland)]. E-mail: tmroczek@pharmacognosy.org; Ndjoko-Ioset, Karine [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland); Glowniak, Kazimierz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Mietkiewicz-Capala, Agnieszka [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Hostettmann, Kurt [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland)

2006-05-04

From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C{sub 18} column using a gradient elution. Based on MS {sup n} spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide.

Validation of the quality control method for sodium dicloxacillin in Dicloxen capsules

International Nuclear Information System (INIS)

Rodriguez Hernandez, Yaslenis; Perez Navarro, Maikel; Suarez Perez, Yania

2014-01-01

Sodium dicloxacillin is a semi synthetic derivative of the isoxasocyl penicillin group that may appear in oral suspension form and in caplets. For the analysis of the raw materials and the finished products, it is recommended to use high performance liquid chromatography that is an unavailable method at the dicloxen capsule manufacturing lab for the routine analysis of the drug. To develop and to validate a useful ultraviolet spectrophotometry method for the quality control of sodium dicloxacillin in Dicloxen capsules

Evaluation of phenolic content, total flavonoid and survey of antioxidant activity of leaves of Ficus carica and Pterocarya fraxinifolia trees using spectrophotometry and high performance liquid chromatograph methods

Directory of Open Access Journals (Sweden)

Naser Jafari

2015-09-01

Full Text Available In this research, to evaluate the antioxidant activity of leaf Pterocarya fraxinifolia (Juglandaceae and Ficus carica (Moraceae extract were carried out by spectrophotometry and high performance liquid chromatography methods. The leaves of P. fraxinifolia and F. carica were collected from Whitney and Shast Kalate (Golestan, Noor (Mazandaran and Asalem (Guilan forests in Iran. Methanolc extract was used in different experiments. The phenolic compounds (gallic acid, coumaric acid and quercetin were also measured by using high performance liquid chromatography (HPLC method.The maximum IC50 for DPPH radical-scavenging activity (595.12±21.4 μg ml-1 were observed in P. fraxinifolia leaves. According to the inhibition time, phenolic compound (gallic acid, coumaric acid and quercetin in F. carica leaves and gallic acid and coumaric acid were detected of Pterocarya leaves methanol extracts. The maximum amount of gallic acid (78.93 and coumaric acid (8.14 in extracts Pterocarya leaves Asalem and the lowest gallic acid (8.56 and coumaric acid (0.89 milligrams per gram was observed in Ficus leaf of Noor forest. Based on the standard chromatogram retention time of gallic acid (2.383, coumaric acid (3.817 and quercetin (7.217 mg/g was reported. This study showed that soil factors, such as potassium, sodium, phosphorus and nitrogen compounds with antioxidant phenolic extracts of the leaves of both plants there is a significant correlation.

Atmospheric pressure photoionisation : An ionization method for liquid chromatography-mass spectrometry

NARCIS (Netherlands)

Robb, DB; Covey, TR; Bruins, AP

2000-01-01

Atmospheric pressure photoionization (APPI) has been successfully demonstrated to provide high sensitivity to LC-MS analysis. A vacuum-ultraviolet lamp designed for photoionization detection in gas chromatography is used as a source of 10-eV photons. The mixture of samples and solvent eluting from

Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

Science.gov (United States)

Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

2014-10-03

Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-08-22

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Electronic spectral detection in liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Biggs, Wilton R. [ChevronTexaco Chemical Co., P. O. Box 1627, Richmond, CA 94802 (United States); Fetzer, John C. [Fetzpahs Consulting, 1283 Santa Fe St., Hercules, CA 94547 (United States)

2002-07-01

The use of absorbance and fluorescence spectrometers as liquid chromatography detectors is described. These detectors offer sensitive detection that can also identify the peaks in a chromatogram. Many examples, mainly from the separation of polycyclic aromatic hydrocarbons, are given that show the selectivity and usefulness of these detectors. (orig.)

Instrumental liquid chromatography: a practical manual on high-performance liquid chromatographic methods

National Research Council Canada - National Science Library

Parris, N. A

1976-01-01

Available texts on liquid chromatography have tended to emphasize the developments in the theoretical understanding of the technique and methodology or to list numerous applications, complete with experimental details...

Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

Science.gov (United States)

Uysal, Deniz; Karadaş, Cennet; Kara, Derya

2017-05-01

A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

Two-Dimensional Liquid Chromatography Analysis of Polystyrene/Polybutadiene Block Copolymers.

Science.gov (United States)

Lee, Sanghoon; Choi, Heejae; Chang, Taihyun; Staal, Bastiaan

2018-05-15

A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (Styrolux) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene- block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition, and chain architecture. While individual LC analysis, including size exclusion chromatography, interaction chromatography, or liquid chromatography at critical condition, is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homopolystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

Instrument platforms for nano liquid chromatography

Czech Academy of Sciences Publication Activity Database

Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

2015-01-01

Roč. 1421, NOV (2015), s. 2-17 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : nano liquid chromatography * splitless gradient generation * nano LC platforms Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0250900

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

Science.gov (United States)

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

2009-01-01

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

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

Science.gov (United States)

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

2015-05-29

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

UHPLC: The Greening Face of Liquid Chromatography.

Science.gov (United States)

Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

2013-01-01

Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

Implementation of the method for the determination of lactulose (4-O-β-D-Galactopyranosyl-D-Fructofuranose) and HMF (5-hydroxymethyl-2-furaldehyde) in ultra-pasteurized milk (UHT) ultraviolet-visible spectrophotometry

International Nuclear Information System (INIS)

Cardenas Miranda, Jeisson Alberto

2015-01-01

Measurement methods of HMF concentrations and lactulose is implemented and evaluated in low-fat milk (2% fat), subjected to ultra pasteurization process in order to establish indicators of nutritional quality. A protocol is developed for the management of equipment and methodology of the analytical method. The determination methods of HMF and lactulose are validated by ultraviolet visible spectrophotometry. The content of HMF and lactulose is determined in different production batches for 4 months of storage at a temperature of 24 Celsius degrees [es

Uranium determination by UV-Vis spectrophotometry in organic matrix

International Nuclear Information System (INIS)

Iwaki, Leonardo E.O.; Silva, Ieda S.; Oliveira, Luis C.

2013-01-01

Concentrations of uranium in the process samples provide essential information required for nuclear process monitoring. A large number of techniques have been developed to allow uranium determination, but each technique possesses some advantages and disadvantages and cannot be applied without difficulty to all samples. The ultraviolet visible spectrophotometry (UV-Vis) is widely method used in analytical industrial processes due to its simplicity, rapidity, low costs, low generation of analytical waste, easy calibration and operation. In this study, we describe a simple and fast quantification method to determination of a high amount of uranium in organic phase (TBP/kerosene) using UV-Vis spectrophotometry. The process sample was analyzed in UV-Vis and compared with inductively coupled plasma optical emission spectrometry (ICP OES) showing similar results in both methods. The statistical tests (Student-t and Fischer) showed that the both techniques they are equivalent. (author)

Multi-filter spectrophotometry simulations

Science.gov (United States)

Callaghan, Kim A. S.; Gibson, Brad K.; Hickson, Paul

1993-01-01

To complement both the multi-filter observations of quasar environments described in these proceedings, as well as the proposed UBC 2.7 m Liquid Mirror Telescope (LMT) redshift survey, we have initiated a program of simulated multi-filter spectrophotometry. The goal of this work, still very much in progress, is a better quantitative assessment of the multiband technique as a viable mechanism for obtaining useful redshift and morphological class information from large scale multi-filter surveys.

Derivative spectrophotometry for the determination of faropenem in the presence of degradation products: an application for kinetic studies.

Science.gov (United States)

Cielecka-Piontek, Judyta

2013-07-01

A simple and selective derivative spectrophotometric method was developed for the quantitative determination of faropenem in pure form and in pharmaceutical dosage. The method is based on the zero-crossing effect of first-derivative spectrophotometry (λ = 324 nm), which eliminates the overlapping effect caused by the excipients present in the pharmaceutical preparation, as well as degradation products, formed during hydrolysis, oxidation, photolysis, and thermolysis. The method was linear in the concentration range 2.5-300 μg/mL (r = 0.9989) at λ = 341 nm; the limits of detection and quantitation were 0.16 and 0.46 μg/mL, respectively. The method had good precision (relative standard deviation from 0.68 to 2.13%). Recovery of faropenem ranged from 97.9 to 101.3%. The first-order rate constants of the degradation of faropenem in pure form and in pharmaceutical dosage were determined by using first-derivative spectrophotometry. A statistical comparison of the validation results and the observed rate constants for faropenem degradation with these obtained with the high-performance liquid chromatography method demonstrated that both were compatible.

High-performance liquid chromatography on-line coupled to high-field NMR and mass spectrometry for structure elucidation of constituents of Hypericum perforatum L

DEFF Research Database (Denmark)

Hansen, S. H.; Jensen, A. G.; Cornett, Claus

1999-01-01

The on-line separation and structure elucidation of naphthodianthrones, flavonoids, and other constituents of an extract from Hypericum perforatum L, using high performance liquid chromatography (HPLC) coupled on-line with ultraviolet-visible, nuclear magnetic resonance (NMR), and mass spectrometry...... (MS) is described. A conventional reversed-phase HPLC system using ammonium acetate as the buffer substance in the eluent tvas used, and proton NMR spectra were obtained on a 500 MHz NMR instrument. The MS and MS/MS analyses were performed using negative electrospray ionization, In the present study...

Fractionation of fecal neutral steroids by high performance liquid chromatography

International Nuclear Information System (INIS)

Jackson, E.M.; Kloss, C.A.; Weintraub, S.T.; Mott, G.E.

1985-01-01

Fecal neutral steroids were fractionated by high performance liquid chromatography (HPLC) into three major fractions: 5 beta-H, 3-keto steroids; 5 beta-H, 3 beta-hydroxy steroids; and 5 alpha-H and delta 5-3 beta-hydroxy steroids. This separation was achieved in about 10 minutes, with greater than 97% recovery of standards in each fraction. Gas-liquid chromatographic quantitation of fecal steroids fractionated by either HPLC or thin-layer chromatography gave nearly identical results. A method using both C18 reverse phase and silica HPLC to purify radiolabeled sterols is also described

VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis. Program. Summary of reports

International Nuclear Information System (INIS)

2001-01-01

Program and summary of reports of the VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis are performed. The meeting took place 15-19 October, 2001 in Moscow. Many problems of liquid and ion exchange chromatography, capillary electrophoresis, thin-layer chromatography have been discussed extensively. Reports covering properties of sorbents and devices for chromatography are incorporated in the collection [ru

One-pot synthesis of zeolitic imidazolate framework-8/poly (methyl methacrylate-ethyleneglycol dimethacrylate) monolith coating for stir bar sorptive extraction of phytohormones from fruit samples followed by high performance liquid chromatography-ultraviolet detection.

Science.gov (United States)

You, Linna; He, Man; Chen, Beibei; Hu, Bin

2017-11-17

In this work, zeolitic imidazolate framework-8 (ZIF-8)/poly (methyl methacrylate-ethyleneglycol dimethacrylate) (MMA-EGDMA) composite monolith was in situ synthesized on stir bar by one-pot polymerization. Compared with the neat monolith, ZIF-8/poly(MMA-EGDMA) composite monolith has larger surface area and pore volume. It also exhibits higher extraction efficiency for target phytohormones than poly(MMA-EGDMA) monolith and commercial polyethylene glycol (PEG) coated stir bar. Based on it, a method of ZIF-8/poly(MMA-EGDMA) monolith coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detection (HPLC-UV) was established for the analysis of five phytohormones in apple and pear samples. The developed method exhibited low limits of detection (0.11-0.51μg/L), wide linear range (0.5-500μg/L) and good recoveries (82.7-111%), which demonstrated good application potential of the ZIF-8/monolith coated stir bar in trace analysis of organic compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultra Performance Liquid Chromatography Tandem Mass ...

African Journals Online (AJOL)

NICOLAAS

drugs alone.16. After a single oral dose of 120–800 mg of NTB in healthy sub- jects in a fasting state the peak plasma NTB concentration (tmax) was found to be 4–7 h, with a half-life of approximately 9–17 h.17 ... performance liquid chromatography mass spectrometry/mass .... to the likely biological plasma constituents.

Nano-liquid chromatography applied to enantiomers separation.

Science.gov (United States)

Fanali, Salvatore

2017-02-24

This paper presents the state of the art concerning the separation of chiral compounds by means of nano-liquid chromatography (nano-LC). The enantiomers' separation and determination are a subject of fundamental importance in various application fields such as pharmaceutical industry, biomedicine, food, agrochemical etc. Nano-LC is a miniaturized chromatographic technique offering some advantages over conventional ones such as low consumption of mobile phase, sample volume and amount of chiral stationary phase, reduced costs etc. This is reported in the first part of the paper illustrating the features of the nano-LC. In addition, chiral resolution methods are briefly illustrated. Some chiral selectors, used in high-performance liquid chromatography have also been applied in nano-LC including cyclodextrins, glycopeptide antibiotics, modified polysaccharides etc. This is discussed in the second part of the review. Finally some examples of the applications available in literature are reported. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultra-high Performance Liquid Chromatography in Steroid Analysis

OpenAIRE

Salonen, Fanny

2017-01-01

The latest version of liquid chromatography is ultra-high performance (or pressure) chromatography (UHPLC). In the technique, short and narrow-bore columns with particle sizes below 3 µm are used. The extremely high pressure used results in very short analysis times, excellent separation, and good resolution. This makes UHPLC a good choice for steroidal analysis. Steroids are a highly interesting area of study; they can be recognized as biomarkers for several diseases and are a relevant topic...

Far ultraviolet spectrophotometry of BD +28 4211

Science.gov (United States)

Cook, Timothy A.; Cash, Webster; Green, James C.

1991-01-01

The results are reported of a November 1989 rocket flight which recorded a flux-calibrated spectrum of BD +28 4211 from 912 to 1150 A with 1A resolution. BD +28 4211, an SdO-type star, is commonly used as an ultraviolet calibration source in the IUE wavelength band. The present work extends the useful range of this standard shortward of Lyman-alpha. Since previous experiments show marked disparity, this study can be useful in determining a standard in the 912 to 1216 A band.

Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

DEFF Research Database (Denmark)

Corr, J. J.; Larsen, Erik Huusfeldt

1996-01-01

Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes...... fragmentation patterns showing molecular dissociation through an expected common product ion were obtained for the four arsenosugars, Molecular mode detection was utilized for qualitative verification of speciation analysis by high-performance liquid chromatography coupled to inductively coupled plasma mass...

Determination of vitamin K homologues by high-performance liquid chromatography with on-line photoreactor and peroxyoxalate chemiluminescence detection

International Nuclear Information System (INIS)

Ahmed, Sameh; Kishikawa, Naoya; Nakashima, Kenichiro; Kuroda, Naotaka

2007-01-01

A sensitive and highly selective high-performance liquid chromatography (HPLC) method was developed for the determination of vitamin K homologues including phylloquinone (PK), menaquinone-4 (MK-4) and menaquinone-7 (MK-7) in human plasma using post-column peroxyoxalate chemiluminescence (PO-CL) detection following on-line ultraviolet (UV) irradiation. The method was based on ultraviolet irradiation (254 nm, 15 W) of vitamin K to produce hydrogen peroxide and a fluorescent product at the same time, which can be determined with PO-CL detection. The separation of vitamin K by HPLC was accomplished isocratically on an ODS column within 35 min. The method involves the use of 2-methyl-3-pentadecyl-1,4-naphthoquinone as an internal standard. The detection limits (signal-to-noise ratio = 3) were 32, 38 and 85 fmol for PK, MK-4 and MK-7, respectively. The recoveries of PK, MK-4 and MK-7 were greater than 82% and the inter- and intra-assay R.S.D. values were 1.9-5.4%. The sensitivity and selectivity of this method were sufficient for clinical and nutritional applications

Analysis of short-chain acids from anaerobic bacteria by high-performance liquid chromatography.

OpenAIRE

Guerrant, G O; Lambert, M A; Moss, C W

1982-01-01

A standard mixture of 25 short-chain fatty acids was resolved by high-performance liquid chromatography, using an Aminex HPX-87 column. The acids produced in culture media by anaerobic bacteria were analyzed by high-performance liquid chromatography after extraction with ether and reextraction into a small volume of 0.1 N NaOH. The presence of fumaric acid in culture extracts of Peptostreptococcus anaerobius was confirmed by gas chromatography-mass spectrometry analysis of the trapped eluent ...

Screening anti-tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry.

Science.gov (United States)

Zhang, Tao; Ding, Yuanyuan; An, Hongli; Feng, Liuxin; Wang, Sicen

2015-07-14

Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine-HEK293 cells were used as cell membrane stationary phase. Specificity and reproducibility of the cell membrane chromatography was evaluated using 1-tert-butyl-3-{2-[4-(diethylamino)butylamino]-6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-7-yl}urea, Nimodipine and dexamethasone acetate. Then, anti-tumor components acting on Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high-performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide-formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose-dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two-dimensional high-performance liquid chromatography method can screen and identify potential anti-tumor ingredients which specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

High-throughput determination of vancomycin in human plasma by a cost-effective system of two-dimensional liquid chromatography.

Science.gov (United States)

Sheng, Yanghao; Zhou, Boting

2017-05-26

Therapeutic drug monitoring (TDM) is one of the most important services of clinical laboratories. Two main techniques are commonly used: the immunoassay and chromatography method. We have developed a cost-effective system of two-dimensional liquid chromatography with ultraviolet detection (2D-LC-UV) for high-throughput determination of vancomycin in human plasma that combines the automation and low start-up costs of the immunoassay with the high selectivity and sensitivity of the liquid chromatography coupled with mass spectrometric detection without incurring their disadvantages, achieving high cost-effectiveness. This 2D-LC system offers a large volume injection to provide sufficient sensitivity and uses simulated gradient peak compression technology to control peak broadening and to improve peak shape. A middle column was added to reduce the analysis cycle time and make it suitable for high-throughput routine clinical assays. The analysis cycle time was 4min and the peak width was 0.8min. Compared with other chromatographic methods that have been developed, the analysis cycle time and peak width for vancomycin was reduced significantly. The lower limit of quantification was 0.20μg/mL for vancomycin, which is the same as certain LC-MS/MS methods that have been recently developed and validated. The method is rapid, automated, and low-cost and has high selectivity and sensitivity for the quantification of vancomycin in human plasma, thus making it well-suited for use in hospital clinical laboratories. Copyright © 2017 Elsevier B.V. All rights reserved.

Ion exchange and liquid column chromatography

International Nuclear Information System (INIS)

Walton, H.F.

1980-01-01

Major accomplishments in liquid chromatography for the past two years and reported in journals available to December 31, 1979 are reviewed. Emphasis has been placed on principles and methodology with some representative examples of application included. Applications are illustrated in two rather lenghtly tables, one covering inorganic ions and the other covering organic compounds. 544 references, 8 books, and 15 reviews are listed in the bibliography

Validated High Performance Liquid Chromatography Method for ...

African Journals Online (AJOL)

Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

Spillage detector for liquid chromatography systems

Science.gov (United States)

Jarvis, M. J.; Fulton, D. S. (Inventor)

1986-01-01

A spillage detector device for use in conjunction with fractionation of liquid chromatography systems which includes a spillage recieving enclosure beneath the fractionation area is described. A sensing device having a plurality of electrodes of alternating polarity is mounted within the spillage recieving enclosure. Detection circuitry, responsive to conductivity between electrodes, is operatively connected to the sensing device. The detection circuitry feeds into the output circuitry. The output circuit has relaying and switching circuitry directed to a solenoid, an alarm system and a pump. The solenoid is connected to the pliable conduit of the chromatography system. The alarm system comprises an audio alarm and a visual signal. A 115-volt power system interconnected with the pump, the solenoid, the sensing device, and the detection and output circuitry.

Instrumental analysis

Energy Technology Data Exchange (ETDEWEB)

Kim, Seung Jae; Seo, Seong Gyu

1995-03-15

This textbook deals with instrumental analysis, which consists of nine chapters. It has Introduction of analysis chemistry, the process of analysis and types and form of the analysis, Electrochemistry on basic theory, potentiometry and conductometry, electromagnetic radiant rays and optical components on introduction and application, Ultraviolet rays and Visible spectrophotometry, Atomic absorption spectrophotometry on introduction, flame emission spectrometry and plasma emission spectrometry. The others like infrared spectrophotometry, X-rays spectrophotometry and mass spectrometry, chromatography and the other instrumental analysis like radiochemistry.

Instrumental analysis

International Nuclear Information System (INIS)

Kim, Seung Jae; Seo, Seong Gyu

1995-03-01

This textbook deals with instrumental analysis, which consists of nine chapters. It has Introduction of analysis chemistry, the process of analysis and types and form of the analysis, Electrochemistry on basic theory, potentiometry and conductometry, electromagnetic radiant rays and optical components on introduction and application, Ultraviolet rays and Visible spectrophotometry, Atomic absorption spectrophotometry on introduction, flame emission spectrometry and plasma emission spectrometry. The others like infrared spectrophotometry, X-rays spectrophotometry and mass spectrometry, chromatography and the other instrumental analysis like radiochemistry.

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

Science.gov (United States)

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

2017-08-01

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

Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

Energy Technology Data Exchange (ETDEWEB)

Campos, Reinaldo C. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil)], E-mail: rccampos@puc-rio.br; Goncalves, Rodrigo A.; Brandao, Geisamanda P.; Azevedo, Marlo S. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil); Oliveira, Fabiana; Wasserman, Julio [Institut of Geosciences, Fluminense Federal University, Av. Gal. Milton Tavares de Souza, s/n, 24.210-340, Niteroi, Rio de Janeiro (Brazil)

2009-06-15

The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C{sub 18} column was used as stationary phase, and post column treatment was performed by UV irradiation (60 deg. C, 13 W). The eluate was then merged with 3 mol L{sup -1} HCl, reduction was performed by a NaBH{sub 4} solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 {mu}g L{sup -1} were obtained for ionic (Hg{sup 2+}) and HgCH{sub 3}{sup +}, for an injection volume of 200 {mu}L. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sedi0011men.

Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

International Nuclear Information System (INIS)

Campos, Reinaldo C.; Goncalves, Rodrigo A.; Brandao, Geisamanda P.; Azevedo, Marlo S.; Oliveira, Fabiana; Wasserman, Julio

2009-01-01

The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C 18 column was used as stationary phase, and post column treatment was performed by UV irradiation (60 deg. C, 13 W). The eluate was then merged with 3 mol L -1 HCl, reduction was performed by a NaBH 4 solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 μg L -1 were obtained for ionic (Hg 2+ ) and HgCH 3 + , for an injection volume of 200 μL. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sediments.

Overview of online two-dimensional liquid chromatography based on cell membrane chromatography for screening target components from traditional Chinese medicines.

Science.gov (United States)

Muhammad, Saqib; Han, Shengli; Xie, Xiaoyu; Wang, Sicen; Aziz, Muhammad Majid

2017-01-01

Cell membrane chromatography is a simple, specific, and time-saving technique for studying drug-receptor interactions, screening of active components from complex mixtures, and quality control of traditional Chinese medicines. However, the short column life, low sensitivity, low column efficiency (so cannot resolve satisfactorily mixture of compounds), low peak capacity, and inefficient in structure identification were bottleneck in its application. Combinations of cell membrane chromatography with multidimensional chromatography such as two-dimensional liquid chromatography and high sensitivity detectors like mass have significantly reduced many of the above-mentioned shortcomings. This paper provides an overview of the current advances in online two-dimensional-based cell membrane chromatography for screening target components from traditional Chinese medicines with particular emphasis on the instrumentation, preparation of cell membrane stationary phase, advantages, and disadvantages compared to alternative approaches. The last section of the review summarizes the applications of the online two-dimensional high-performance liquid chromatography based cell membrane chromatography reported since its emergence to date (2010-June 2016). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Beta-induced fluorescence detection in liquid chromatography

International Nuclear Information System (INIS)

Malcolme-Lawes, D.J.; Massey, S.; Warwick, P.

1981-01-01

A theoretical analysis of beta-induced fluorescence is used to determine the factors which influence the sensitivity of the technique as applied to liquid chromatography. Equations are presented for detector response and for signal-to-noise ratios and the theoretical response for a typical detector is compared with experimentally determined values. (author)

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

Directory of Open Access Journals (Sweden)

Lei-Wen Xiang

2014-04-01

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

Microchip-based monolithic column for high performance liquid chromatography

Data.gov (United States)

National Aeronautics and Space Administration — We have developed microchip based monolithic columns that can be used for liquid chromatography of small organic molecules, as well as, macromolecules such as...

Polypyrrole-magnetite dispersive micro-solid-phase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater.

Science.gov (United States)

Kamaruddin, Amirah Farhan; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Md Shukri, Dyia S; Abdul Keyon, Aemi S

2017-11-01

Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R 2  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations extraction and determination of dyes at trace concentration levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A high performance liquid chromatography method for determination of furfural in crude palm oil.

Science.gov (United States)

Loi, Chia Chun; Boo, Huey Chern; Mohammed, Abdulkarim Sabo; Ariffin, Abdul Azis

2011-09-01

A modified steam distillation method was developed to extract furfural from crude palm oil (CPO). The collected distillates were analysed using high performance liquid chromatography (HPLC) coupled with an ultraviolet diode detector at 284nm. The HPLC method allowed identification and quantification of furfural in CPO. The unique thermal extraction of CPO whereby the fresh fruit bunches (FFB) are first subjected to steam treatment, distinguishes itself from other solvent-extracted or cold-pressed vegetable oils. The presence of furfural was also determined in the fresh palm oil from FFB (without undergoing the normal extraction process), palm olein, palm stearin, olive oil, coconut oil, sunflower oil, soya oil and corn oil. The chromatograms of the extracts were compared to that of standard furfural. Furfural was only detected in CPO. The CPO consignments obtained from four mills were shown to contain 7.54 to 20.60mg/kg furfural. Copyright © 2011 Elsevier Ltd. All rights reserved.

High-performance liquid chromatography of oligoguanylates at high pH

Science.gov (United States)

Stribling, R.; Deamer, D. (Principal Investigator)

1991-01-01

Because of the stable self-structures formed by oligomers of guanosine, standard high-performance liquid chromatography techniques for oligonucleotide fractionation are not applicable. Previously, oligoguanylate separations have been carried out at pH 12 using RPC-5 as the packing material. While RPC-5 provides excellent separations, there are several limitations, including the lack of a commercially available source. This report describes a new anion-exchange high-performance liquid chromatography method using HEMA-IEC BIO Q, which successfully separates different forms of the guanosine monomer as well as longer oligoguanylates. The reproducibility and stability at high pH suggests a versatile role for this material.

A generalized theory of chromatography and multistep liquid extraction

Science.gov (United States)

Chizhkov, V. P.; Boitsov, V. N.

2017-03-01

A generalized theory of chromatography and multistep liquid extraction is developed. The principles of highly efficient processes for fine preparative separation of binary mixture components on a fixed sorbent layer are discussed.

The Assessment of Liver Reserve Function by Spectrophotometry based on Determination of Phenacetin and Paracetamol.

Science.gov (United States)

Ren, Rui; Ma, Yongmei; Ma, Wanshan; Lu, Sumei

2015-01-01

To establish a technical system for assessing liver reserve function based on spectrophotometry by detection of phenacetin and paracetamol in blood samples. Taking detected contents of phenacetin and paracetamol by high performance liquid chromatography (HPLC) as standard, which was proved to be able to detect drug concentrations with high resolution and accuracy, we established a technical system based on the spectrophotometric technique to assay phenacetin and paracetamol, including the color system, the maximum absorption wavelength, the influence factors of color system, and the optimal conditions for hydrolysis. Then we verified our established system compared with that under HPLC by recovery test. This study established a technical system to detect phenacetin and paracetamol in blood samples using spectrophotometry. Mainly, 3 mol/L hydrochloric acid (HCl) was added to samples for hydrolysis for 30 minutes, then, adding 0.02% 1,2-naphthoquinone-4-sulfonate (NQS), 1% cetyltrimethyl ammonium bromide (CTA) and 2% sodium hydroxide (or 3% sodium carbonate) (ratio of 1:6:1:2 or 3), and the absorbance was measured at 500 nm and 570 nm to calculate their concentrations. Using an established spectrophotometric system to detect phenacetin and paracetamol in blood samples could assess liver reserve function, which was proved comparable with HPLC in resolution and repeatability.

Comparison of two novel in-syringe dispersive liquid-liquid microextraction techniques for the determination of iodide in water samples using spectrophotometry.

Science.gov (United States)

Kaykhaii, Massoud; Sargazi, Mona

2014-01-01

Two new, rapid methodologies have been developed and applied successfully for the determination of trace levels of iodide in real water samples. Both techniques are based on a combination of in-syringe dispersive liquid-liquid microextraction (IS-DLLME) and micro-volume UV-Vis spectrophotometry. In the first technique, iodide is oxidized with nitrous acid to the colorless anion of ICl2(-) at high concentration of hydrochloric acid. Rhodamine B is added and by means of one step IS-DLLME, the ion-pair formed was extracted into toluene and measured spectrophotometrically. Acetone is used as dispersive solvent. The second method is based on the IS-DLLME microextraction of iodide as iodide/1, 10-phenanthroline-iron((II)) chelate cation ion-pair (colored) into nitrobenzene. Methanol was selected as dispersive solvent. Optimal conditions for iodide extraction were determined for both approaches. Methods are compared in terms of analytical parameters such as precision, accuracy, speed and limit of detection. Both methods were successfully applied to determining iodide in tap and river water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2000-08-11

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

Clinical applications of fast liquid chromatography: a review on the analysis of cardiovascular drugs and their metabolites.

Science.gov (United States)

Baranowska, Irena; Magiera, Sylwia; Baranowski, Jacek

2013-05-15

One of the major challenges facing the medicine today is developing new therapies that enhance human health. To help address these challenges the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality. In the last decade various analytical strategies have been established to enhance separation speed and efficiency in liquid chromatography applications. Liquid chromatography is an increasingly important tool for monitoring drugs and their metabolites. Furthermore, liquid chromatography has played an important role in pharmacokinetics and metabolism studies at these drug development stages since its introduction. This paper provides an overview of current trends in fast chromatography for the analysis of cardiovascular drugs and their metabolites in clinical applications. Current trends in fast liquid chromatographic separations involve monolith technologies, fused-core columns, high-temperature liquid chromatography (HTLC) and ultra-high performance liquid chromatography (UHPLC). The high specificity in combination with high sensitivity makes it an attractive complementary method to traditional methodology used for routine applications. The practical aspects of, recent developments in and the present status of fast chromatography for the analysis of biological fluids for therapeutic drug and metabolite monitoring, pharmacokinetic studies and bioequivalence studies are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

Application of Ionic Liquids in High Performance Reversed-Phase Chromatography

Directory of Open Access Journals (Sweden)

Wentao Bi

2009-06-01

Full Text Available Ionic liquids, considered “green” chemicals, are widely used in many areas of analytical chemistry due to their unique properties. Recently, ionic liquids have been used as a kind of novel additive in separation and combined with silica to synthesize new stationary phase as separation media. This review will focus on the properties and mechanisms of ionic liquids and their potential applications as mobile phase modifier and surface-bonded stationary phase in reversed-phase high performance liquid chromatography (RP-HPLC. Ionic liquids demonstrate advantages and potential in chromatographic field.

Ultra high performance liquid chromatography of seized drugs

NARCIS (Netherlands)

Lurie, I.S.

2010-01-01

The primary goal of this thesis is to investigate the use of ultra high performance liquid chromatography (UHPLC) for the analysis of seized drugs. This goal was largely achieved and significant progress was made in achieving improved separation and detection of drugs of forensic interest.

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

Science.gov (United States)

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

2015-07-01

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

Identification and spectrophotometry of faint southern radio galaxies

International Nuclear Information System (INIS)

Spinrad, H.; Kron, R.G.; Hunstead, R.W.

1980-01-01

We have observed a mixed sample of southern radio sources, identified on the Palomar sky survey or on previous direct plates taken with medium-aperture reflectors. At CIO we obtained a few deep 4m photographs and SIT spectrophotometry for redshift and continuum-color measurement. Almost all our sources were faint galaxies; the largest redshift measured was for 3C 275, with z=0.480. The ultraviolet continuum of PKS 0400--643, a ''thermal'' galaxy with z=0.476, closely resembles that of 3C 295 and shows some color evolution in U--B compared to nearby giant ellipticals

Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

DEFF Research Database (Denmark)

Harrison, I.; Leader, R.U.; Higgo, J.J.W.

1994-01-01

A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after neu...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

Mallow carotenoids determined by high-performance liquid chromatography

Science.gov (United States)

Mallow (corchorus olitorius) is a green vegetable, which is widely consumed either fresh or dry by Middle East population. This study was carried out to determine the contents of major carotenoids quantitatively in mallow, by using a High Performance Liquid Chromatography (HPLC) equipped with a Bis...

Recent advances in ultra-high performance liquid chromatography for the analysis of traditional chinese medicine

Science.gov (United States)

Traditional Chinese medicines (TCMs) have been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra Performance Liquid Chromatography (UHPLC) is a relatively new technique offering new possibilities in liquid chromatography. This paper reviews recen...

Purification Efficacy of Synthetic Cannabinoid Conjugates Using High-Pressure Liquid Chromatography

Science.gov (United States)

conducted using high-pressure liquid chromatography and gradient screens to determine the most effective means of purifying the SC:dark quencher conjugates...to obtain the highest yields and purity. The purity was verified using liquid chromatographycoupled mass spectroscopy and nuclear magnetic resonance.

Comparison of ultra-violet and inductively coupled plasma-atomic emission spectrometry for the on-line quantification of selenium species after their separation by reversed-phase liquid chromatography

International Nuclear Information System (INIS)

Tsopelas, Fotios N.; Ochsenkuehn-Petropoulou, Maria Th.; Mergias, Ioannis G.; Tsakanika, Lambrini V.

2005-01-01

An analytical approach for selenium speciation using liquid chromatography (LC) coupled with ultra-violet (UV) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed. The separation of the investigated selenium species, selenites, selenates, selenomethionine, selenocystine, selenocystamine and dimethyldiselenide was accomplished in less than 6 min on a BIO Wide Pore RP-18 column using sodium salt of n-octanesulfonic acid as ion-pairing modifier. The on-line detection of the separated selenium species was performed using UV spectrometry at the optimum wavelength of 192 nm, obtained by the UV spectra of the investigated individual selenium species. ICP-AES was also used as element specific on-line detector, after its coupling with the chromatographic system. The UV and ICP-AES detectors were compared for their suitability, including sensitivity and detection limits, for the on-line quantification of the six selenium species. The developed LC-UV as well as LC-ICP-AES techniques were successfully applied to a selenized yeast candidate reference material, after its enzymatic extraction with protease XIV. It was found that the described LC-UV technique is suitable for the determination of selenomethionine, the main selenium compound in the yeast, with an accuracy of 5%, although the UV detector is not element specific and it is rarely used for selenium speciation. This finding can prove valuable for routine laboratories to perform selenium speciation in such materials

Csaba Horváth and preparative liquid chromatography.

Science.gov (United States)

Guiochon, Georges

2005-06-24

Few chromatographers have been interested in furthering preparative liquid chromatography. The pioneers, Tswett, Kuhn and Lederer, A.J.P. Martin, Tiselius, isolated fractions but as an intermediate step in the analysis of their samples. The progress in electronics and sensors, and in their miniaturization has lead to the paradoxical situation that the analysts never see the transient pure fractions that their detector quantitates. Yet, over the last 25 years, preparative liquid chromatography has become an important industrial process for the separation, the extraction, and/or the purification of many pharmaceuticals or pharmaceutical intermediates, including pure enantiomers, purified peptides and proteins, compounds that are manufactured at the relatively large industrial scale of a few kilograms to several hundred tons per year. This development that has strongly affected the modem pharmaceutical industry is mainly due to the pioneering work of Csaba Horváth. His work in preparative HPLC was critical at both the practical and the theoretical levels. He was the first scientist in modem times to pay serious attention to the relationships between the curvature of the equilibrium isotherms, the competitive nature of nonlinear isotherms, and the chromatographic band profiles of complex mixtures. The thermodynamics of multi-component phase equilibria and mass transfer kinetics in chromatography attracted his interest and were the focus of ground-breaking contributions. He investigated displacement chromatography, an old method invented by Tiselius that Csaba was first to implement in HPLC. This choice was explained by the essential characteristic of displacement chromatography, in that it delivers fractions that can be far more concentrated than the feed. Remarkably, once the basics of nonlinear chromatography had been mastered in his group, most of the applications that were studied by his coworkers dealt with peptides of various sizes and with proteins. Thus, all

Separation of Poly(styrene-block-t-butyl methacrylate) Copolymers by Various Liquid Chromatography Techniques

Science.gov (United States)

Šmigovec Ljubič, Tina; Pahovnik, David; Žigon, Majda; Žagar, Ema

2012-01-01

The separation of a mixture of three poly(styrene-block-t-butyl methacrylate) copolymers (PS-b-PtBMA), consisting of polystyrene (PS) blocks of similar length and t-butyl methacrylate (PtBMA) blocks of different lengths, was performed using various chromatographic techniques, that is, a gradient liquid chromatography on reversed-phase (C18 and C8) and normal-phase columns, a liquid chromatography under critical conditions for polystyrene as well as a fully automated two-dimensional liquid chromatography that separates block copolymers by chemical composition in the first dimension and by molar mass in the second dimension. The results show that a partial separation of the mixture of PS-b-PtBMA copolymers can be achieved only by gradient liquid chromatography on reversed-phase columns. The coelution of the two block copolymers is ascribed to a much shorter PtBMA block length, compared to the PS block, as well as a small difference in the length of the PtBMA block in two of these copolymers, which was confirmed by SEC-MALS and NMR spectroscopy. PMID:22489207

Chemistry and liquid chromatography methods for the analyses of primary oxidation products of triacylglycerols.

Science.gov (United States)

Zeb, A

2015-05-01

Triacylglycerols (TAGs) are one of the major components of the cells in higher biological systems, which can act as an energy reservoir in the living cells. The unsaturated fatty acid moiety is the key site of oxidation and formation of oxidation compounds. The TAG free radical generates several primary oxidation compounds. These include hydroperoxides, hydroxides, epidioxides, hydroperoxy epidioxides, hydroxyl epidioxides, and epoxides. The presence of these oxidized TAGs in the cell increases the chances of several detrimental processes. For this purpose, several liquid chromatography (LC) methods were reported in their analyses. This review is therefore focused on the chemistry, oxidation, extraction, and the LC methods reported in the analyses of oxidized TAGs. The studies on thin-layer chromatography were mostly focused on the total oxidized TAGs separation and employ hexane as major solvent. High-performance LC (HPLC) methods were discussed in details along with their merits and demerits. It was found that most of the HPLC methods employed isocratic elution with methanol and acetonitrile as major solvents with an ultraviolet detector. The coupling of HPLC with mass spectrometry (MS) highly increases the efficiency of analysis as well as enables reliable structural elucidation. The use of MS was found to be helpful in studying the oxidation chemistry of TAGs and needs to be extended to the complex biological systems.

Analysis of Fluconazole in Human Urine Sample by High Performance Liquid Chromatography Method

International Nuclear Information System (INIS)

Hermawan, D; Ali, N A Md; Ibrahim, W A Wan; Sanagi, M M

2013-01-01

A method for determination of fluconazole, antifungal drug in human urine by using reversed-phased high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detector was developed. Optimization HPLC conditions were carried out by changing the flow rate and composition of mobile phase. The optimum separation conditions at a flow rate 0.85 mL/min with a composition of mobile phase containing methanol:water (70:30, v/v) with UV detection at a wavelength 254 nm was able to analyze fluconazole within 3 min. The excellent linearity was obtained in the range of concentration 1 to 10 μg/mL with r 2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 μg/mL and 1.28 μg/mL, respectively. Solid phase extraction (SPE) method using octadecylsilane (C18) as a sorbent was used to clean-up and pre-concentrated of the urine sample prior to HPLC analysis. The average recoveries of fluconazole in spiked urine sample was 72.4% with RSD of 3.21% (n=3).

Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

Science.gov (United States)

Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

2016-03-01

A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Quality evaluation of moluodan concentrated pill using high-performance liquid chromatography fingerprinting coupled with chemometrics.

Science.gov (United States)

Tao, Lingyan; Zhang, Qing; Wu, Yongjiang; Liu, Xuesong

2016-12-01

In this study, a fast and effective high-performance liquid chromatography method was developed to obtain a fingerprint chromatogram and quantitative analysis simultaneously of four indexes including gallic acid, chlorogenic acid, albiflorin and paeoniflorin of the traditional Chinese medicine Moluodan Concentrated Pill. The method was performed by using a Waters X-bridge C 18 reversed phase column on an Agilent 1200S high-performance liquid chromatography system coupled with diode array detection. The mobile phase of the high-performance liquid chromatography method was composed of 20 mmol/L phosphate solution and acetonitrile with a 1 mL/min eluent velocity, under a detection temperature of 30°C and a UV detection wavelength of 254 nm. After the methodology validation, 16 batches of Moluodan Concentrated Pill were analyzed by this high-performance liquid chromatography method and both qualitative and quantitative evaluation results were achieved by similarity analysis, principal component analysis and hierarchical cluster analysis. The results of these three chemometrics were in good agreement and all indicated that batch 10 and batch 16 showed significant differences with the other 14 batches. This suggested that the developed high-performance liquid chromatography method could be applied in the quality evaluation of Moluodan Concentrated Pill. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ion-exclusion/cation-exchange chromatography with dual detection of the conductivity and spectrophotometry for the simultaneous determination of common inorganic anionic species and cations in river and wastewater.

Science.gov (United States)

Nakatani, Nobutake; Kozaki, Daisuke; Mori, Masanobu; Hasebe, Kiyoshi; Nakagoshi, Nobukazu; Tanaka, Kazuhiko

2011-01-01

Simultaneous determinations of common inorganic anionic species (SO(4)(2-), Cl(-), NO(3)(-), phosphate and silicate) and cations (Na(+), NH(4)(+), K(+), Mg(2+) and Ca(2+)) were conducted using an ion-chromatography system with dual detection of conductivity and spectrophotometry in tandem. The separation of ionic species on a weakly acidic cation-exchange resin was accomplished using a mixture of 100 mM ascorbic acid and 4 mM 18-crown-6 as an acidic eluent (pH 2.6), after which the ions were detected using a conductivity detector. Subsequently, phosphate and silicate were analyzed based on derivatization with molybdate and spectrophotometry at 700 nm. The detection limits at S/N = 3 ranged from 0.11 to 2.9 µM for analyte ionic species. This method was applied to practical river water and wastewater with acceptable criteria for the anion-cation balance and comparisons of the measured and calculated electrical conductivity, demonstrating the usefulness of the present method for water quality monitoring.

Fiber-based monolithic columns for liquid chromatography.

Science.gov (United States)

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.

Salt-induced phase separation for the determination of metals as their diethyldithiocarbamate complexes by high-performance liquid chromatography

International Nuclear Information System (INIS)

Mueller, B.J.; Lovett, R.J.

1987-01-01

Reversed-phase high-performance liquid chromatography with ultraviolet detection can be used to determine trace levels of Pt(II), Pd(II), Rh(III), Co(III), Ru(III), and Ir in aqueous solution following complexation with diethyldithiocarbamate. The metal complexes are extracted into acetonitrile from aqueous solution by the addition of a saturated salt solution. Quantitative metal recovery from aqueous solution is achievable for most metals for a wide solution pH range. Detection limits for the metals are <3 ng of metal/mL of original aqueous sample. Analyses of real samples are highly reproducible and sensitive. Ir an interfere in the determination of Pt(II) and Rh(III). A general protocol for chromatographic separation and determination of Pt(II), Pd(II), Rh(III), Ru(III), and Ir in aqueous solution is presented

Liquid chromatography - mass spectrometry analysis of pharmaceuticals

International Nuclear Information System (INIS)

Macasek, F.

2003-01-01

The drugs represent mostly non-volatile and thermally labile solutes, often available only in small amounts like it is in case of radiopharmaceuticals. Therefor, the favourable separation techniques for such compounds are HPLC, capillary electrophoresis and also TLC 1. Liquid chromatography with mass spectrometric detector (LC/MS) is especially powerful for their microanalysis. Mass spectrometry separating the ions in high vacuum was presumably used as detector for gas chromatography effluent but the on-line coupling with liquid eluant flow 0.1-1 mL/min is far more challenging. New types of ion sources were constructed for simultaneous removal of solvent and ionisation of solutes at atmospheric pressure (API). At present, a relatively wide choice of successfully designed commercial equipment is available either for small organic molecules and larger biomolecules (Perkin-Elmer, Agilent, Jeol, Bruker Daltonics, ThermoQuest, Shimadzu). The features of the LC/MS systems are presented. LC/MS as a new quality control tool for [F-18]fluorodeoxyglucose (FDG) radiopharmaceutical, which has became the most spread radiopharmaceutical for positron emission tomography (PET), was proposed. Other applications of the LC/MS are reviewed. (author)

Analysis of metalaxyl racemate using high performance liquid chromatography coupled with four kinds of detectors.

Science.gov (United States)

Chen, Tao; Fan, Jun; Gao, Ruiqi; Wang, Tai; Yu, Ying; Zhang, Weiguang

2016-10-07

Chiral stationary phase-high performance liquid chromatography coupled with various detectors has been one of most commonly used methods for analysis and separation of chiral compounds over the past decades. Various detectors exhibit different characteristics in qualitative and quantitative studies under different chromatographic conditions. Herein, a comparative evaluation of HPLC coupled with ultraviolet, optical rotation, refractive index, and evaporative light scattering detectors has been conducted for qualitative and quantitative analyses of metalaxyl racemate. Effects of separation conditions on the peak area ratio between two enantiomers, including sample concentration, column temperature, mobile phase composition, as well as flow rate, have been investigated in detail. In addition, the limits of detection, the limits of quantitation, quantitative range and precision for these two enantiomers by using four detectors have been also studied. As indicated, the chromatographic separation conditions have been slight effects on ultraviolet and refractive index detections and the peak area ratio between two enantiomers remains almost unchanged, but the evaporative light scattering detection has been significantly affected by the above-mentioned chromatographic conditions and the corresponding peak area ratios varied greatly. Moreover, the limits of detection, the limits of quantitation, and the quantitative ranges of two enantiomers with UV detection were remarkably lower by 1-2 magnitudes than the others. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2017-06-08

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

Combined high-performance liquid chromatography/32P-postlabeling assay of N7-methyldeoxyguanosine

International Nuclear Information System (INIS)

Shields, P.G.; Povey, A.C.; Wilson, V.L.; Weston, A.; Harris, C.C.

1990-01-01

A highly sensitive and specific assay for the detection of N7-methyl-2'-deoxyguanosine (N7methyldG) has been developed by combining high-performance liquid chromatography, 32 P-postlabeling, and nucleotide chromatography. Separation of normal nucleotides and adducts by high-performance liquid chromatography and then combining a portion of 2'-deoxyguanosine to the N7methyldG allows for quantitation using an internal standard. The directly determined molar ratio is not subject to errors in digestion, variable ATP-specific activity, or assumptions in relative adduct-labeling efficiency. The detection limit was one N7methyldG adduct in 10(7) unmodified 2'-deoxyguanosine bases. N7methyldG adducts have been detected in 5 human lung samples in which O6-methyl-2'-deoxyguanosine adducts had been previously determined. The mean ratio of N7methyldG to O6-methyl-2'-deoxyguanosine was determined to be approximately 10. The current assay complements the high-performance liquid chromatography/ 32 P-postlabeling assay for O6-methyl-2'-deoxyguanosine and increases the detection sensitivity of DNA methylated by exogenous alkylating agents

High Performance Liquid Chromatography of Vitamin A: A Quantitative Determination.

Science.gov (United States)

Bohman, Ove; And Others

1982-01-01

Experimental procedures are provided for the quantitative determination of Vitamin A (retinol) in food products by analytical liquid chromatography. Standard addition and calibration curve extraction methods are outlined. (SK)

Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

OpenAIRE

Suriyavathana Muthukrishnan; Subha Palanisamy; Senthilkumar Subramanian; Sumathi Selvaraj; Kavitha Rani Mari; Ramalingam Kuppulingam

2016-01-01

Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. Th...

(Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

International Nuclear Information System (INIS)

Mokhtarani, Babak; Gmehling, Juergen

2010-01-01

(Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

(Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Mokhtarani, Babak [Chemistry and Chemical Engineering Research Center of Iran, P.O. Box 14335-186, Tehran (Iran, Islamic Republic of); Gmehling, Juergen, E-mail: gmehling@tech.chem.uni-oldenburg.d [Carl von Ossietzky Universitaet Oldenburg, Technische Chemie, D-26111 Oldenburg (Germany)

2010-08-15

(Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

Improvement of mineral oil saturated and aromatic hydrocarbons determination in edible oil by liquid-liquid-gas chromatography with dual detection.

Science.gov (United States)

Zoccali, Mariosimone; Barp, Laura; Beccaria, Marco; Sciarrone, Danilo; Purcaro, Giorgia; Mondello, Luigi

2016-02-01

Mineral oils, which are mainly composed of saturated hydrocarbons and aromatic hydrocarbons, are widespread food contaminants. Liquid chromatography coupled to gas chromatography with flame ionization detection represents the method of choice to determine these two families. However, despite the high selectivity of this technique, the presence of olefins (particularly squalene and its isomers) in some samples as in olive oils, does not allow the correct quantification of the mineral oil aromatic hydrocarbons fraction, requiring additional off-line tools to eliminate them. In the present research, a novel on-line liquid chromatography coupled to gas chromatography method is described for the determination of hydrocarbon contamination in edible oils. Two different liquid chromatography columns, namely a silica one (to retain the bulk of the matrix) and a silver-ion one (which better retains the olefins), were coupled in series to obtain the mineral oil aromatic hydrocarbons hump free of interfering peaks. Furthermore, the use of a simultaneous dual detection, flame ionization detector and triple quadrupole mass spectrometer allowed us not only to quantify the mineral oil contamination, but also to evaluate the presence of specific markers (i.e. hopanes) to confirm the petrogenic origin of the contamination. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comprehensive two-dimensional liquid chromatography with on-line Fourier-transform-infrared-spectroscopy detection for the characterization of copolymers

NARCIS (Netherlands)

Kok, S.J.; Hankemeier, T.; Schoenmakers, P.J.

2005-01-01

The on-line coupling of comprehensive two-dimensional liquid chromatography (liquid chromatography × size-exclusion chromatography, LC × SEC) and infrared (IR) spectroscopy has been realized by means of an IR flow cell. The system has been assessed by the functional-group analysis of a series of

Thin-layer chromatography - liquid chromatography, an ideal supplement demonstrated by the separation of lanthanoids

International Nuclear Information System (INIS)

Specker, H.; Hufnagel, A.

1984-01-01

All lanthanoids have been separated by thin-layer chromatography (TLC) with short retention times by using a mixture of ether/tetrahydrofurane (THF)/bis-(2-ethylhexyl)-phosphate (HDEHP)/nitric acid. The eluent was empirically tested by synergistic effects. The results have been transferred to high-performance liquid chromatography /HPLC). It was possible to use the same eluent in TLC and HPLC both for the analytical separation of all lanthanoids and for the separation of fission products. The experimental experience gained in HPLC could be applied to the pre-concentration of isotopes in TLC. Both methods excellently supplemented each other in the separation of lanthanoids. (orig.) [de

The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Johnson, Steven [Iowa State Univ., Ames, IA (United States)

1999-02-12

The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

Characterization of porous silicon integrated in liquid chromatography chips

NARCIS (Netherlands)

Tiggelaar, Roald M.; Verdoold, Vincent; Eghbali, H.; Desmet, G.; Gardeniers, Johannes G.E.

2009-01-01

Properties of porous silicon which are relevant for use of the material as a stationary phase in liquid chromatography chips, like porosity, pore size and specific surface area, were determined with high-resolution SEM and N2 adsorption–desorption isotherms. For the anodization conditions

Effect of Ultraviolet Aging on Rheology and Chemistry of LDH-Modified Bitumen

Directory of Open Access Journals (Sweden)

Xing Liu

2015-08-01

Full Text Available Layered double hydroxides (LDHs are an ultravioletlight (UV-resistant material. In this study, two types of LDHs (Mg-Al-LDHs and Zn-Al-LDHs were applied to modify bitumen by melt-blending. The effect of ultraviolet aging on the rheology and chemistry of LDH-modified bitumen was studied by means of dynamic shear rheometer (DSR, thin-layer chromatography with flame ionization detection (TLC-FID, Fourier transform infrared spectroscopy (FTIR, and Ultraviolet-Visible (UV-Vis spectrophotometry to reveal the mechanisms of action for LDHs and bitumen. The results showed that within the UV spectra (220–400 nm, the reflectance of Zn-Al-LDHs was larger than that of Mg-Al-LDHs. These two LDHs have different influences on the performance of bitumen. Mg-Al-LDHs had a more obvious influence on the physical and dynamic rheological properties of bitumen than Zn-Al-LDHs. Zn-Al-LDHs improved the UV-aging resistance of bitumen more. The reason can be that the reflectance of the Zn-Al-LDHs to the UV light is larger than that of the Mg-Al-LDHs. The Zn-Al-LDH-modified bitumen had more potential to improve the UV-aging resistance during the service life of asphalt pavement.

Determination of carbamazepine in serum and saliva samples by high performance liquid chromatography with ultraviolet detection.

Science.gov (United States)

Dordević, Snezana; Kilibarda, Vesna; Stojanović, Tomislav

2009-05-01

Carbamazepine is antiepileptic drug widely used for the treatment of epilepsy. Due to low therapeutic index of carbamazepine there is a need for routine measuring its concentrations in biological fluids. The aim of the study was to describe a method for concomitant determination of carbamazepine in the serum and saliva. Separation of the drug from matrix is achieved by reversed-phase chromatography on a C18 column, with a mobile phase of methanol-water-acetic acid (65:34:1) at a flow-rate of 1.0 ml/min. Detection was effected by ultra-violet absorption at 285 nm. The total run time was 5 min. Samples were prepared by alkaline extraction (pH 10) using chlorophorm. Calibration curves were in the range 0.1-5 microg/mL for serum and saliva samples. Mean recoveries of spiked serum and saliva were 97.59 and 92.30%, respectively. Limits of detection (LOD) of carbamazepine in serum and saliva were 0.166 and 0.178 microg/mL, respectively. Limits of quantification (LOQ) in the serum and saliva were 0.237 and 0.226 microg/mL, respectively. The method precision was carried out with coefficient of variation of 2.10% and 4.03% for the serum and saliva, respectively. The obtained data showed that there was a strong correlation between saliva and serum concentrations (r = 0.9481, p < 0.001). The method described here is rapid, precise, accurate and simple, and can be used for quantitative determination of carbamazepine in human serum and saliva after therapy applying. Saliva samples could be used as an alternative matrix for therapeutic drug monitoring of this antiepileptic drug.

Determination of methylphenidate in Calliphorid larvae by liquid-liquid extraction and liquid chromatography mass spectrometry - Forensic entomotoxicology using an in vivo rat brain model

DEFF Research Database (Denmark)

Bushby, Sarah K.; Thomas, Nicky; Priemel, Petra A.

2012-01-01

and Calliphorid larvae) by liquid-liquid extraction with recovery of >80%, and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS assay was validated for entomotoxicological use and initially applied to male Sprague-Dawley rats (n=6) that were dosed with MPH (20mg/kg) ante...

Method transfer from high-pressure liquid chromatography to ultra-high-pressure liquid chromatography. II. Temperature and pressure effects.

Science.gov (United States)

Åsberg, Dennis; Samuelsson, Jörgen; Leśko, Marek; Cavazzini, Alberto; Kaczmarski, Krzysztof; Fornstedt, Torgny

2015-07-03

The importance of the generated temperature and pressure gradients in ultra-high-pressure liquid chromatography (UHPLC) are investigated and compared to high-pressure liquid chromatography (HPLC). The drug Omeprazole, together with three other model compounds (with different chemical characteristics, namely uncharged, positively and negatively charged) were used. Calculations of the complete temperature profile in the column at UHPLC conditions showed, in our experiments, a temperature difference between the inlet and outlet of 16 °C and a difference of 2 °C between the column center and the wall. Through van't Hoff plots, this information was used to single out the decrease in retention factor (k) solely due to the temperature gradient. The uncharged solute was least affected by temperature with a decrease in k of about 5% while for charged solutes the effect was more pronounced, with k decreases up to 14%. A pressure increase of 500 bar gave roughly 5% increase in k for the uncharged solute, while omeprazole and the other two charged solutes gave about 25, 20 and 15% increases in k, respectively. The stochastic model of chromatography was applied to estimate the dependence of the average number of adsorption/desorption events (n) and the average time spent by a molecule in the stationary phase (τs) on temperature and pressure on peak shape for the tailing, basic solute. Increasing the temperature yielded an increase in n and decrease in τs which resulted in less skew at high temperatures. With increasing pressure, the stochastic modeling gave interesting results for the basic solute showing that the skew of the peak increased with pressure. The conclusion is that pressure effects are more pronounced for both retention and peak shape than the temperature effects for the polar or charged compounds in our study. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Owens, J; Hok, S; Alcaraz, A; Koester, C

2008-11-13

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

Quantitative Analysis of Tetramethylenedisulfotetramine ('Tetramine') Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

International Nuclear Information System (INIS)

Owens, J.; Hok, S.; Alcaraz, A.; Koester, C.

2008-01-01

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 50 = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 (micro)g/mL by LC/MS/MS versus 0.15 (micro)g/mL for GC/MS. Fortifications of the beverages at 2.5 (micro)g/mL and 0.25 (micro)g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

Simultaneous analysis of tert-butylhydroquinone, tert-butylquinone, butylated hydroxytoluene, 2-tert-butyl-4-hydroxyanisole, 3-tert-butyl-4-hydroxyanisole, α-tocopherol, γ-tocopherol, and δ-tocopherol in edible oils by normal-phase high performance liquid chromatography.

Science.gov (United States)

Li, Jun; Bi, Yanlan; Sun, Shangde; Peng, Dan

2017-11-01

A normal-phase high performance liquid chromatography method for the simultaneous determination of tert-butylhydroquinone, tert-butylquinone, butylated hydroxytoluene, 2-tert-butyl-4-hydroxyanisole, 3-tert-butyl-4-hydroxyanisole, α-tocopherol, γ-tocopherol, and δ-tocopherol in edible oils was investigated. A silica column was used to separate the analytes with the gradient elution. An ultraviolet-visible detector was set at dual wavelengths mode (280 and 310nm). The column temperature was 30°C. The analytes were directly extracted with methanol. Results showed that the normal-phase high performance liquid chromatography method performed well with wide liner ranges (0.10∼500.00μg/mL, R 2 >0.9998), low limits of detection and quantitation (below 0.40 and 1.21μg/mL, respectively), and good recoveries (81.38∼102.34% in soybean oils and 83.03∼100.79% in lard, respectively). The reduction of tert-butylquinone caused by the reverse-phase high performance liquid chromatography during the injection was avoided with the current normal-phase method. The two isomers of butylated hydroxyanisole can also be separated with good resolution. Copyright © 2017 Elsevier Ltd. All rights reserved.

Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

Science.gov (United States)

Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

2016-06-17

This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultraviolet energy distributions and the temperatures of peculiar B and A stars

International Nuclear Information System (INIS)

Adelman, S.J.; NASA, Goddard Space Flight Center, Greenbelt, MD)

1985-01-01

Color temperatures have been estimated by comparing ultraviolet observations of HgMn and magnetic Ap stars with those of normal stars. Ultraviolet data from the OAO-2, ANS, TD-1, and IUE satellites generally give similar results. The values for the normal stars were derived from comparison of fluxes predicted by solar-composition fully line-blanketed model atmospheres with optical region spectrophotometry. The ultraviolet temperatures of the HgMn stars cover a narrower temperature range than do their optical region values. Magnetic Ap stars with similar optical region temperatures can show substantial differences in their ultraviolet color temperatures. This may result from magnetic field configuration and abundance differences. 27 references

Rapid Screening and Characterization of Acetylcholinesterase Inhibitors from Yinhuang Oral Liquid Using Ultrafiltration-liquid Chromatography-electrospray Ionization Tandem Mass Spectrometry.

Science.gov (United States)

Zhang, Haomin; Guo, Yinan; Meng, Lingwen; Sun, Hui; Yang, Yinping; Gao, Ying; Sun, Jiaming

2018-01-01

At present, approximately 17-25 million people in the world suffer from Alzheimer's disease (AD). The most efficacious and acceptable therapeutic drug clinically are the acetylcholinesterase inhibitors (AChEIs). Yinhuang oral liquid is a Chinese medicine preparation which contains AChEIs according to the literatures. However, no strategy has been presented for rapid screening and identification of AChEIs from Yinhuang oral liquid. To develop a method for rapid screening and identification of AChEIs from Yinhuang oral liquid using ultrafiltration-liquid chromatography-electrospray ionization tandem mass spectrometry (UF-LC-ESI-MS/MS). In this study, UF incubation conditions such as enzyme concentration, incubation time, and incubation temperature were optimized so as to get better screening results. The AChEIs from Yinhuang oral liquid were identified by high-performance liquid chromatography-ESI-MS and the improved Ellman method was used for the AChE inhibitory activity test in vitro . The results showed that Yinhuang oral liquid can inhibit the activity of AChE. We screened and identified seven compounds with potential AChE inhibitory activity from Yinhuang oral liquid, which provided experimental basis for the treatment and prevention of AD. The current technique was used to directly screen the active ingredients with acetylcholinesterase inhibition from complex traditional Chinese medicine, which was simple, rapid, accurate, and suitable for high-throughput screening of AChEI from complex systems. A UF-LC-ESI-MS/MS method for rapid screening and identification of AChEIs from Yinhuang oral liquid was developedSeven compounds were screened and identified with potential AChE inhibitory activity from Yinhuang oral liquidIt provided experimental basis of Yinhuang oral liquid for the treating and preventing AD. Abbreviations used: (AD): Alzheimer's disease; (UF-LC-ESI-MS/MS): ultrafiltration-liquid chromatography-electrospray ionization tandem mass spectrometry; (ACh

Monitoring aged reversed-phase high performance liquid chromatography columns

NARCIS (Netherlands)

Bolck, A; Smilde, AK; Bruins, CHP

1999-01-01

In this paper, a new approach for the quality assessment of routinely used reversed-phase high performance liquid chromatography columns is presented. A used column is not directly considered deteriorated when changes in retention occur. If attention is paid to the type and magnitude of the changes,

Nanomaterials as stationary phases and supports in liquid chromatography.

Science.gov (United States)

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

2017-10-01

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

Recent advances in liquid and gas chromatography methodology for extending coverage of the metabolome.

Science.gov (United States)

Haggarty, Jennifer; Burgess, Karl Ev

2017-02-01

The metabolome is the complete complement of metabolites (small organic biomolecules). In order to comprehensively understand the effect of stimuli on a biological system, it is important to detect as many of the metabolites within that system as possible. This review briefly describes some new advances in liquid and gas chromatography to improve coverage of the metabolome, including the serial combination of two columns in tandem, column switching and different variations of two-dimensional chromatography. Supercritical fluid chromatography could provide complimentary data to liquid and gas chromatography. Although there have been many recent advancements in the field of metabolomics, it is evident that a combination, rather than a single method, is required to approach full coverage of the metabolome. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

Parallel artificial liquid membrane extraction of acidic drugs from human plasma

DEFF Research Database (Denmark)

Roldan-Pijuan, Mercedes; Pedersen-Bjergaard, Stig; Gjelstad, Astrid

2015-01-01

The new sample preparation concept “Parallel artificial liquid membrane extraction (PALME)” was evaluated for extraction of the acidic drugs ketoprofen, fenoprofen, diclofenac, flurbiprofen, ibuprofen, and gemfibrozil from human plasma samples. Plasma samples (250 μL) were loaded into individual......-performance liquid chromatography-ultraviolet detection of the individual acceptor solutions. Important PALME parameters including the chemical composition of the liquid membrane, extraction time, and sample pH were optimized, and the extraction performance was evaluated. Except for flurbiprofen, exhaustive...

Quantification of Tea Flavonoids by High Performance Liquid Chromatography

Science.gov (United States)

Freeman, Jessica D.; Niemeyer, Emily D.

2008-01-01

We have developed a laboratory experiment that uses high performance liquid chromatography (HPLC) to quantify flavonoid levels in a variety of commercial teas. Specifically, this experiment analyzes a group of flavonoids known as catechins, plant-derived polyphenolic compounds commonly found in many foods and beverages, including green and black…

Polyaniline/cyclodextrin composite coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the analysis of trace polychlorinated biphenyls in environmental waters.

Science.gov (United States)

Lei, Yun; He, Man; Chen, Beibei; Hu, Bin

2016-04-01

A novel polyaniline/α-cyclodextrin (PANI/α-CD) composite coated stir bar was prepared by sol-gel process for the analysis of polychlorinated biphenyls (PCBs) in this work. The preparation reproducibility of the PANI/α-CD-coated stir bar was good, with relative standard deviations (RSDs) ranging from 2.3% to 3.7% (n=7) and 2.0% to 3.8% (n=7) for bar to bar and batch to batch, respectively. Based on it, a novel method of PANI/α-CD-coated stir bar sorptive extraction (SBSE) followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for the determination of trace PCBs in environmental waters. To obtain the best extraction performance for target PCBs, several parameters affecting SBSE, such as extraction time, stirring rate, and ionic strength were investigated. Under optimal experimental conditions, the limits of detection (LODs) of the proposed method for seven PCBs were in the range of 0.048-0.22 μg/L, and the RSDs were 5.3-9.8% (n=7, c=1 μg/L). Enrichment factors (EFs) ranging from 39.8 to 68.4-fold (theoretical EF, 83.3-fold) for target analytes were achieved. The proposed method was successfully applied for the determination of seven target PCBs in Yangtze River water and East Lake water, and the recoveries were in the range of 73.0-120% for the spiked East Lake water samples and 82.7-121% for the spiked Yangtze River water samples, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

The high pressure electronic control system in liquid chromatography

International Nuclear Information System (INIS)

Popescu, Stefan; Popeneciu, Gabriel; Toadere, Florin

2002-01-01

The Liquid Chromatography system can perform a wide variety of measurements and separations especially for the organic liquids, with maximum applications flexibility for less than half price of Gas Chromatography. The repeatability and accuracy of results in quantitative high pressure liquid chromatography are highly dependent on the reproducibility and accuracy of both integrated flow rate and mobile phase composition. Flow rate fluctuation leads to poor reproducibility in both integrated peak areas and retention times. Similarly, poor control of mobile phase composition will cause poor repeatability of retention time and peak heights. The our Solvent Delivery System SDS 200 is a single pump system which provides precise compensated flow rates from 0.01 to 10 mL/min, selectable upper pressure limits of 0 to 100 bar or 10 to 450 bar, and solvent compressibility correction. Ternary solvent system on-line mixing capability saves time, reduces solvent waste and provides more flexibility for difficult separations. The pump itself has two different displacement pistons which are used alternately on both suction and discharge, so that intake of the solvent are synchronous. The evacuated solvent from the two pump's chambers is mixed in the reference unit and then is supplied to the damping unit for flow ripple reduction. The SDS Electronic Module ensures the functions: controls the programmed flow rate, detects and shows the solvent pressure in solvent, supplies the step motor, measures and limits the solvent pressure. The control panel of SDS 200, contains a two-stages flow decimal programmer, a eight-positions knob for upper pressure limits, an alarm LED and a parallel port for connection to a PC system. (authors)

Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques.

Science.gov (United States)

Engida, Adam Mekonnen; Faika, Sitti; Nguyen-Thi, Bich Thuyen; Ju, Yi-Hsu

2015-06-01

In the present work, heat reflux extraction with ethanol/water (80:20; v/v) as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE) was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF) and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1) were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut. Copyright © 2014. Published by Elsevier B.V.

Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques

Directory of Open Access Journals (Sweden)

Adam Mekonnen Engida

2015-06-01

Full Text Available In the present work, heat reflux extraction with ethanol/water (80:20; v/v as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1 were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut.

Amphenicols stability in medicated feed – development and validation of liquid chromatography method

Directory of Open Access Journals (Sweden)

Pietro Wojciech Jerzy

2014-12-01

Full Text Available A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF and thiamphenicol (TAP in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3 on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm analytical column with UV (λ = 220 nm detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.

Monodisperse microbeads of hypercrosslinked polystyrene for liquid and supercritical fluid chromatography

Science.gov (United States)

Tsyurupa, M. P.; Blinnikova, Z. K.; Il'in, M. M.; Davankov, V. A.; Parenago, O. O.; Pokrovskii, O. I.; Usovich, O. I.

2015-11-01

Monodisperse styrene-divinylbenzene (1 wt %) copolymer microbeads are obtained via the elaborate method of high-productivity precipitation polymerization. The crosslinking of this copolymer with chloromethyl methyl ether in the presence of Friedel-Crafts catalyst yields porous hypercrosslinked polymers with degrees of crosslinking that range from 200 to 500%. Microbead sorbents are shown to be suited for selective stationary phases for high-performance liquid chromatography and supercritical fluid chromatography.

Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

Science.gov (United States)

Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

2016-08-01

Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Symbiotic stars: spectrophotometry at 3-4 and 8-13 μm

International Nuclear Information System (INIS)

Roche, P.F.; Aitken, D.K.

1983-01-01

Infrared spectrophotometry of 20 symbiotic stars, mostly of dust-rich variety, is presented. HDE 330036 is unique in showing an emission feature at 11.3 μm. The remainder combine a hot grey component and/or optically thin silicate emission. A model in which the grey component is due to optically thick silicate dust is not consistent with the spectra. It is proposed instead that iron-based grains, expected to form in the ejecta of cool stars, are heated by the ultraviolet radiation field of the hot companion. (author)

A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

Science.gov (United States)

Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

2016-02-01

It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

Science.gov (United States)

DiNunzio, James E.

1985-01-01

Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

Determination of chlormequat in pears by liquid chromatography/mass spectrometry

NARCIS (Netherlands)

Mol, H.G.J.; Dam, R.C.J. van; Vreeken, R.J.; Steijger, O.M.

2000-01-01

A straightforward and reliable method was developed for the determination of chlormequat in pears by liquid chromatography/mass spectrometry (LC/MS). Water and methanol were compared as extraction solvents. Because no significant differences in extraction efficiency or repeatability were found,

Sensitive determination of nitrophenol isomers by reverse-phase high-performance liquid chromatography in conjunction with liquid-liquid extraction

Science.gov (United States)

A method for the highly sensitive determination of 2-, 3- and 4- nitrophenols was developed using reverse-phase high-performance liquid chromatography (RP-HPLC) with a UV photodiode array detector. Using a reverse-phase column and 40% aqueous acetonitrile as an eluent (i.e. isocratic elution), the i...

Determination of carbamazepine in serum and saliva samples by high performance liquid chromatography with ultraviolet detection

Directory of Open Access Journals (Sweden)

Đorđević Snežana

2009-01-01

Full Text Available Background/Aim. Carbamazepine is antiepileptic drug widely used for the treatment of epilepsy. Due to low therapeutic index of carbamazepine there is a need for routine measuring its concentrations in biological fluids. The aim of the study was to describe a method for concomitant determination of carbamazepine in the serum and saliva. Methods. Separation of the drug from matrix is achieved by reversedphase chromatography on a C18 column, with a mobile phase of methanol-water-acetic acid (65:34:1 at a flow-rate of 1.0 ml/min. Detection was effected by ultra-violet absorption at 285 nm. The total run time was 5 min. Samples were prepared by alkaline extraction (pH 10 using chlorophorm. Results. Calibration curves were in the range 0.1-5 μg/mL for serum and saliva samples. Mean recoveries of spiked serum and saliva were 97.59 and 92.30%, respectively. Limits of detection (LOD of carbamazepine in serum and saliva were 0.166 and 0.178 μg/mL, respectively. Limits of quantification (LOQ in the serum and saliva were 0.237 and 0.226 μg/mL, respectively. The method precision was carried out with coefficient of variation of 2.10% and 4.03% for the serum and saliva, respectively. The obtained data showed that there was a strong correlation between saliva and serum concentrations (r = 0.9481, p < 0.001. Conclusion. The method described here is rapid, precise, accurate and simple, and can be used for quantitative determination of carbamazepine in human serum and saliva after therapy applying. Saliva samples could be used as an alternative matrix for therapeutic drug monitoring of this antiepileptic drug.

Atomic-fluorescence spectrophotometry

International Nuclear Information System (INIS)

Bakhturova, N.F.; Yudelevich, I.G.

1975-01-01

Atomic-fluorescence spectrophotometry, a comparatively new method for the analysis of trace quantities, has developed rapidly in the past ten years. Theoretical and experimental studies by many workers have shown that atomic-fluorescence spectrophotometry (AFS) is capable of achieving a better limit than atomic absorption for a large number of elements. The present review examines briefly the principles of atomic-fluorescence spectrophotometry and the types of fluorescent transition. The excitation sources, flame and nonflame atomizers, used in AFS are described. The limits of detection achieved up to the present, using flame and nonflame methods of atomization are given

Characterization of natural organic colorants in historical and art objects by high-performance liquid chromatography.

Science.gov (United States)

Pauk, Volodymyr; Barták, Petr; Lemr, Karel

2014-12-01

High-performance liquid chromatography plays an important role in analysis of historical organic colorants. A number of papers have been published in this field over the last 30 years. Classification of the most commonly used natural dyes and an overview of high-performance liquid chromatography methods with main focus on recent works (2008 to the beginning of 2014) are provided. The review deals with an entire analytical protocol covering sample preparation, chromatographic separation, and suitable detection (UV/visible and fluorescent spectroscopy and mass spectrometric techniques). High-performance liquid chromatography has been successfully used in the complete characterization of some organic dyestuffs present in historical and art objects. The possibilities and difficulties for identification of natural sources of historical colorants are also discussed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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.

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

Process of quantity determination of uranium by chromatography in liquid zone

International Nuclear Information System (INIS)

Muller, J.P.; Cojean, J.; Daubizit, M.

1993-01-01

The invention concerns a process of quantity determination of uranium by chromatography in liquid zone, usable to determine the quantity of uranium traces. Solutions to be treated can be aqueous or organic

Evaluation between ultrahigh pressure liquid chromatography and high-performance liquid chromatography analytical methods for characterizing natural dyestuffs.

Science.gov (United States)

Serrano, Ana; van Bommel, Maarten; Hallett, Jessica

2013-11-29

An evaluation was undertaken of ultrahigh pressure liquid chromatography (UHPLC) in comparison to high-performance liquid chromatography (HPLC) for characterizing natural dyes in cultural heritage objects. A new UHPLC method was optimized by testing several analytical parameters adapted from prior UHPLC studies developed in diverse fields of research. Different gradient elution programs were tested on seven UHPLC columns with different dimensions and stationary phase compositions by applying several mobile phases, flow rates, temperatures, and runtimes. The UHPLC method successfully provided more improved data than that achieved by the HPLC method. Indeed, even though carminic acid has shown circa 146% higher resolution with HPLC, UHPLC resulted in an increase of 41-61% resolution and a decrease of 91-422% limit of detection, depending on the dye compound. The optimized method was subsequently assigned to analyse 59 natural reference materials, in which 85 different components were ascribed with different physicochemical properties, in order to create a spectral database for future characterization of dyes in cultural heritage objects. The majority of these reference samples could be successfully distinguished with one single method through the examination of these compounds' retention times and their spectra acquired with a photodiode array detector. These results demonstrate that UHPLC analyses are extremely valuable for the acquisition of more precise chromatographic information concerning natural dyes with complex mixtures of different and/or closely related physicochemical properties, essential for distinguishing similar species of plants and animals used to colour cultural heritage objects. Copyright © 2013 Elsevier B.V. All rights reserved.

Applications of the solvation parameter model in reversed-phase liquid chromatography.

Science.gov (United States)

Poole, Colin F; Lenca, Nicole

2017-02-24

The solvation parameter model is widely used to provide insight into the retention mechanism in reversed-phase liquid chromatography, for column characterization, and in the development of surrogate chromatographic models for biopartitioning processes. The properties of the separation system are described by five system constants representing all possible intermolecular interactions for neutral molecules. The general model can be extended to include ions and enantiomers by adding new descriptors to encode the specific properties of these compounds. System maps provide a comprehensive overview of the separation system as a function of mobile phase composition and/or temperature for method development. The solvation parameter model has been applied to gradient elution separations but here theory and practice suggest a cautious approach since the interpretation of system and compound properties derived from its use are approximate. A growing application of the solvation parameter model in reversed-phase liquid chromatography is the screening of surrogate chromatographic systems for estimating biopartitioning properties. Throughout the discussion of the above topics success as well as known and likely deficiencies of the solvation parameter model are described with an emphasis on the role of the heterogeneous properties of the interphase region on the interpretation and understanding of the general retention mechanism in reversed-phase liquid chromatography for porous chemically bonded sorbents. Copyright © 2016 Elsevier B.V. All rights reserved.

Optimization of the combination micro-high-performance liquid-chromatography/mass spectrometry

International Nuclear Information System (INIS)

Haider, K.

1997-03-01

The coupling of liquid chromatography and mass spectrometry is still growing in significance. In this thesis, a particle beam interface has been investigated for combining ion chromatography with mass spectrometric detection. To introduce the eluent directly (without membrane suppressor) into the spectrometer, only methods with low flow rates like microcolumn chromatography can be used. For the preparation of the columns, reversed-phase and silica-based anion exchange materials were packed into PEEK, steel and fused-silica capillaries with i.d. from 130 to 1000 μm using different methods. The performance of the particle beam interface (modified with a new miniaturized aerosol generator) and the mass spectrometric detection has been studied for a series of inorganic anions as well as aminopolycarboxylic acids and the metal-EDTA complexes. Detection limits between 10 and 100 ng injected could be achieved in the multiple ion detection mode of the mass spectrometer for the investigated solutes. A second type of interface, the direct liquid introduction (DLI) has been used to analyze the priority pollutant phenols. This interface is based on a modified GC-interface into the MS. Separation columns used so far include packed fused-silica capillaries with inner diameter of 75 μm and polystyrene-divinylbenzene (functionalized with tert. butyl groups) as stationary phase. Aspects of instrumentation and effects of chemical ionization in the direct liquid introduction mode are discussed. (author)

Liquid chromatography-mass spectrometry coupling by the intermediary of a liquid micro chromatography-electro spray interface; Couplage chromatographie liquide-spectrometrie de masse par l`intermediaire d`une interface electrospray-microchromatographie liquide

Energy Technology Data Exchange (ETDEWEB)

Gillard Factor, C

1996-12-06

The objective of this work is to realize a liquid chromatography- mass spectrometry coupling by the intermediary of an electro spray interface and the evaluation of performances of tis analytical tool to study pollutants in water, and more particularly pesticides whom maximum admissible concentration in a table water is 0.1{mu}g/l. This study has allowed to bring to the fore the interest of the ionization mode by electro spray in a LC/MS coupling to identify and quantify pesticides in the state of traces without treating the sample. Then, it was demonstrated the usefulness of this analytical tool to detect high molecular masses molecules. (N.C.)

Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry.

Science.gov (United States)

Nielen, M W; Buijtenhuijs, F A

1999-05-01

Hyphenation of liquid chromatography (LC) techniques with electrospray ionization (ESI) orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS) provides both MS-based structural information and LC-based quantitative data in polymer analysis. In one experimental setup, three different LC modes are interfaced with MS:  size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS). In SEC/MS, both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra are achieved. GPEC/MS shows detailed chemical heterogeneity of the polymer and the chemical composition distribution within oligomer groups. In LCCC/MS, the retention behavior is primarily governed by chemical heterogeneities, such as different end group functionalities, and quantitative end group calculations can be easily made. The potential of these methods and the benefit of time-of-flight analyzers in polymer analysis are discussed using SEC/MS of a polydisperse poly(methyl methacrylate) sample, GPEC/MS of dipropoxylated bisphenol A/adipic acid polyester resin, LCCC/MS of alkylated poly(ethylene glycol), and LCCC/MS of terephthalic acid/neopentyl glycol polyester resin.

Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

Science.gov (United States)

Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

Assay for dihydroorotase using high-performance liquid chromatography with radioactivity detection

International Nuclear Information System (INIS)

Mehdi, S.; Wiseman, J.S.

1989-01-01

An assay for measuring dihydroorotase activity was devised. Radiolabeled substrate and product were separated by high-performance liquid chromatography using a reverse-phase column with ion-pairing, and the radioactivity was quantitated by flow detection

Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

DEFF Research Database (Denmark)

Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

2010-01-01

. The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

Determination of trimethyllead reference material using high performance liquid chromatography-inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Lu Hai; Wei Chao; Wang Jun; Chao Jingbo; Zhou Tao; Chen Dazhou

2005-01-01

A high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) was combined, and the chromatography conditions were optimized. The stability and homogeneity of a trimethyllead reference material were determined using this method. (authors)

Combined derivatization and high-performance liquid chromatography with fluorescence and ultraviolet detection for simultaneous analysis of octreotide and gabexate mesylate metabolite in human pancreatic juice samples.

Science.gov (United States)

Carlucci, Giuseppe; Selvaggi, Federico; Sulpizio, Sara; Bassi, Claudio; Carlucci, Maura; Cotellese, Roberto; Ferrone, Vincenzo; Innocenti, Paolo; Locatelli, Marcello

2015-06-01

A simple and sensitive method based on the combination of derivatization and high-performance liquid chromatography with ultraviolet and fluorimetric detection was developed for the simultaneous determination of octreotide and gabexate mesylate metabolite in human pancreatic juice samples. Parameters of the derivatization procedure affecting extraction efficiency were optimized. The developed method was validated according to the International Conference on Harmonization guidelines. The calibration curves were linear over a range of 0.1-15 µg/mL for octreotide and 0.20-15 µg/mL for gabexate mesylate metabolite. Derivatized products of octreotide and gabexate mesylate metabolite were separated on a Luna C18 column (4.6 × 250 mm; 5 µm particle size) using a gradient with a run time of 36 min, without further purification. The limits of detection were 0.025 and 0.05, respectively, for octreotide and gabexate mesylate metabolite. This paper reports the validation of a quantitative high performance liquid chromatography-photodiode array-fluorescence (HPLC-PDA-FL) method for the simultaneous analysis of octreotide and gabexate mesylate metabolite in pancreatic juice by protein precipitation using zinc sulfate-methanol-acetonitrile containing the derivatizing reagent, 4-fluoro-7-nitro-[2,1,3]-benzoxadiazole (NBD-F). Derivatized products of octreotide and gabexate mesylate metabolite were separated on a Luna C18 column (4.6 × 250 mm; 5 µm particle size) using a gradient with a run time of 36 min, without further purification. The method was validated over the concentration ranges 0.1-15 and 0.2-15 µg/mL for octreotide and gabexate mesylate metabolite, respectively, in human pancreatic juice. Biphalin and methyl-p-hydroxybenzoate were used as the internal standards. This method was successfully utilized to support clinical studies in humans. The results from assay validations show that the method is selective, sensitive and robust. The limit

Stationary and through-flow radiochemical detectors in cooperation with high performance liquid chromatography: Application in biochemistry

International Nuclear Information System (INIS)

Kehr, J.

1986-01-01

A review article is presented containing some original experimental data and discussing the usability of radiochemical detection of labelled compounds using high performance liquid chromatography. The stationary and through-flow types of detection are compared with respect to efficiency, chromatographic zone resolution, usability in biochemical research, and also to the current trends of development of liquid chromatography. (author). 3 figs., 1 tab., 19 refs

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

Directory of Open Access Journals (Sweden)

Jean Wan Hong Yong

2017-03-01

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

Cromatografia unificada Unified chromatography

Directory of Open Access Journals (Sweden)

Carin von Mühlen

2004-10-01

Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

Immunoaffinity chromatography of abscisic acid combined with electrospray liquid chromatography–mass spectrometry

Czech Academy of Sciences Publication Activity Database

Hradecká, Veronika; Novák, Ondřej; Havlíček, Libor; Strnad, Miroslav

2007-01-01

Roč. 847, č. 2 (2007), s. 162-173 ISSN 1570-0232 R&D Projects: GA MŠk(CZ) LC06034; GA AV ČR IBS5038351 Institutional research plan: CEZ:AV0Z50380511 Source of funding: V - iné verejné zdroje ; V - iné verejné zdroje Keywords : abscisic acid * immunoaffinity chromatography * liquid chromatography-mass spectrometry Subject RIV: ED - Physiology Impact factor: 2.935, year: 2007

Superparamagnetic graphene oxide-based dispersive-solid phase extraction for preconcentration and determination of tamsulosin hydrochloride in human plasma by high performance liquid chromatography-ultraviolet detection.

Science.gov (United States)

Pashaei, Yaser; Ghorbani-Bidkorbeh, Fatemeh; Shekarchi, Maryam

2017-05-26

In the present study, superparamagnetic graphene oxide-Fe 3 O 4 nanocomposites were successfully prepared by a modified impregnation method (MGO mi ) and their application as a sorbent in the magnetic-dispersive solid phase extraction (M-dSPE) mode to the preconcentration and determination of tamsulosin hydrochloride (TMS) in human plasma was investigated by coupling with high performance liquid chromatography-ultraviolet detection (HPLC-UV). The structure, morphology and magnetic properties of the prepared nanocomposites were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and vibrating sample magnetometry (VSM). Some factors affecting the extraction efficiency, including the pH value, amount of sorbent, extraction time, elution solvent and its volume, and desorption time were studied and optimized. Magnetic nanocomposites plasma extraction of TMS following HPLC analyses showed a linear calibration curve in the range of 0.5-50.0ngmL -1 with an acceptable correlation coefficient (R 2 =0.9988). The method was sensitive, with a low limit of detection (0.17ngmL -1 ) and quantification (0.48ngmL -1 ). Inter- and intra-day precision expressed as relative standard deviation (n=3) and the preconcentration factor, were found to be 5.6-7.2%, 2.9-4.2% and 10, respectively. Good recoveries (98.1-101.4%) with low relative standard deviations (4.2-5.0%) indicated that the matrices under consideration do not significantly affect the extraction process. Due to its high precision and accuracy, the developed method may be a HPLC-UV alternative with M-dSPE for bioequivalence analysis of TMS in human plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantification of nimesulide in human plasma by high-performance liquid chromatography with ultraviolet detector (HPLC-UV): application to pharmacokinetic studies in 28 healthy Korean subjects.

Science.gov (United States)

Kim, Mi-Sun; Park, Yoo-Sin; Kim, Shin-Hee; Kim, Sang-Yeon; Lee, Min-Ho; Kim, Youn-Hee; Kim, Do-Wan; Yang, Seok-Chul; Kang, Ju-Seop

2012-05-01

Nimesulide is a selective COX-2 inhibitor that is as effective as the classical non-acidic nonsteroidal anti-inflammatory drugs in the relief of various pain and inflammatory conditions, but is better tolerated with lower incidences of adverse effects than other drugs. After oral dose of 100 mg nimesulide to western subjects, a mean maximal concentration (C(max)) of 2.86 ∼ 6.5 µg/mL was reached at 1.22 ∼ 2.75 h and mean t(1/2β) of 1.8 ∼ 4.74 h. This study developed a robust method for quantification of nimesulide for the pharmacokinetics and suitability of its dosage in Korea and compared its suitability with other racial populations. Nimesulide and internal standard were extracted from acidified samples with methyl tert-butyl ether and analyzed by high-performance liquid chromatography with ultraviolet detection (HPLC-UV). The 28 healthy volunteers took 2 tablets of 100 mg nimesulide and blood concentrations were analyzed during the 24 h post dose. Several pharmacokinetic parameters were represented: AUC(0-infinity) = 113.0 mg-h/mL, C(max) = 12.06 mg/mL, time for maximal concentrations (T(max)) = 3.19 h and t(1/2β) = 4.51 h. These were different from those of western populations as follows: AUC was 14.5% and C(max) was 28% that of of Korean subjects and T(max) and t(1/2β) were also different. The validated HPLC-UV method was successfully applied for the pharmacokinetic studies of nimesulide in Korean subjects. Because the pharmacokinetics of nimesulide were different from western populations, its dosage regimen needs to be adjusted for Koreans. © The Author [2012]. Published by Oxford University Press. All rights reserved.

High-Performance Liquid Chromatography in the Undergraduate Chemical Engineering Laboratory

Science.gov (United States)

Frey, Douglas D.; Guo, Hui; Karnik, Nikhila

2013-01-01

This article describes the assembly of a simple, low-cost, high-performance liquid chromatography (HPLC) system and its use in the undergraduate chemical engineering laboratory course to perform simple experiments. By interpreting the results from these experiments students are able to gain significant experience in the general method of…

Identification and deconvolution of carbohydrates with gas chromatography-vacuum ultraviolet spectroscopy.

Science.gov (United States)

Schenk, Jamie; Nagy, Gabe; Pohl, Nicola L B; Leghissa, Allegra; Smuts, Jonathan; Schug, Kevin A

2017-09-01

Methodology for qualitative and quantitative determination of carbohydrates with gas chromatography coupled to vacuum ultraviolet detection (GC-VUV) is presented. Saccharides have been intently studied and are commonly analyzed by gas chromatography-mass spectrometry (GC-MS), but not always effectively. This can be attributed to their high degree of structural complexity: α/β anomers from their axial/equatorial hydroxyl group positioning at the C1-OH and flexible ring structures that lead to the open chain, five-membered ring furanose, and six-membered ring pyranose configurations. This complexity can result in convoluted chromatograms, ambiguous fragmentation patterns and, ultimately, analyte misidentification. In this study, mono-, di, and tri-saccharides were derivatized by two different methods-permethylation and oximation/pertrimethylsilylation-and analyzed by GC-VUV. These two derivatization methods were then compared for their efficiency, ease of use, and robustness. Permethylation proved to be a useful technique for the analysis of ketopentoses and pharmaceuticals soluble in dimethyl sulfoxide (DMSO), while the oximation/pertrimethylsilylation method prevailed as the more promising, overall, derivatization method. VUV spectra have been shown to be distinct and allow for efficient differentiation of isomeric species such as ketopentoses and reducing versus non-reducing sugars. In addition to identification, pharmaceutical samples containing several compounds were derivatized and analyzed for their sugar content with the GC-VUV technique to provide data for qualitative analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Directory of Open Access Journals (Sweden)

Ambika Chamoli

2016-01-01

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

Application of genetic algorithms for parameter estimation in liquid chromatography

International Nuclear Information System (INIS)

Hernandez Torres, Reynier; Irizar Mesa, Mirtha; Tavares Camara, Leoncio Diogenes

2012-01-01

In chromatography, complex inverse problems related to the parameters estimation and process optimization are presented. Metaheuristics methods are known as general purpose approximated algorithms which seek and hopefully find good solutions at a reasonable computational cost. These methods are iterative process to perform a robust search of a solution space. Genetic algorithms are optimization techniques based on the principles of genetics and natural selection. They have demonstrated very good performance as global optimizers in many types of applications, including inverse problems. In this work, the effectiveness of genetic algorithms is investigated to estimate parameters in liquid chromatography

Column liquid chromatography applied to concentrating, separating, and determining platinum metals

International Nuclear Information System (INIS)

Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

1986-01-01

The present survey deals with high-performance liquid chromatography (HPLC) in relation to the chromatographic behavior of the platinum metals, including separation and determination. The data shows that HPLC is the most promising and effective method of separating metals, including platinum ones. The method provides efficient separation of microgram amoounts of mixtures with a resolving power 3-20 times that of thin-layer chromatography. It is shown that the most promising line of advance in HPLC for inorganic systems lies in the separation and determination of metals as chelates by absorption or ion-pair chromatography. Examples of using HPLC for determining noble metals in particular cases indicate that the metrological characteristics are favorable

Integration of electrochemistry with ultra-performance liquid chromatography/mass spectrometry.

Science.gov (United States)

Cai, Yi; Zheng, Qiuling; Liu, Yong; Helmy, Roy; Loo, Joseph A; Chen, Hao

2015-01-01

This study presents the development of ultra-performance liquid chromatography (UPLC) mass spectrometry (MS) combined with electrochemistry (EC) for the first time and its application for the structural analysis of proteins/peptides that contain disulfide bonds. In our approach, a protein/peptide mixture sample undergoes a fast UPLC separation and subsequent electrochemical reduction in an electrochemical flow cell followed by online MS and tandem mass spectrometry (MS/MS) analyses. The electrochemical cell is coupled to the mass spectrometer using our recently developed desorption electrospray ionization (DESI) interface. Using this UPLC/EC/DESI-MS method, peptides that contain disulfide bonds can be differentiated from those without disulfide bonds, as the former are electroactive and reducible. MS/MS analysis of the disulfide-reduced peptide ions provides increased information on the sequence and disulfide-linkage pattern. In a reactive DESI- MS detection experiment in which a supercharging reagent was used to dope the DESI spray solvent, increased charging was obtained for the UPLC-separated proteins. Strikingly, upon online electrolytic reduction, supercharged proteins (e.g., α-lactalbumin) showed even higher charging, which will be useful in top- down protein structure MS analysis as increased charges are known to promote protein ion dissociation. Also, the separation speed and sensitivity are enhanced by approximately 1(~)2 orders of magnitude by using UPLC for the liquid chromatography (LC)/EC/MS platform, in comparison to the previously used high- performance liquid chromatography (HPLC). This UPLC/EC/DESI-MS method combines the power of fast UPLC separation, fast electrochemical conversion, and online MS structural analysis for a potentially valuable tool for proteomics research and bioanalysis.

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

Science.gov (United States)

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

2013-01-01

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

Carbon nanoparticles from corn stalk soot and its novel application as stationary phase of hydrophilic interaction chromatography and per aqueous liquid chromatography

International Nuclear Information System (INIS)

Li Yuanyuan; Xu Luan; Chen Tong; Liu Xiaoyan; Xu Zhigang; Zhang Haixia

2012-01-01

Highlights: ► Carbon nanoparticles (6–18 nm in size) were prepared from corn stalk soot. ► CNPs-based silica were used as novel chromatography stationary phase. ► The new phase shows good separation selectivity for polar compounds. ► The new phase had the similar retention for polar probes in HILIC and PALC modes. ► In contrast to PALC, under HILIC conditions high efficiencies were achieved. - Abstract: Carbon nanoparticles (CNPs) (6–18 nm in size) were prepared by refluxing corn stalk soot in nitric acid. The obtained acid-oxidized CNPs are soluble in water due to the existence of carboxylic and hydroxyl groups. 13 C NMR measurement shows the CNPs are mainly of sp 2 and sp 3 carbon structure different from CNPs obtained from candle soot and natural gas soot. Furthermore, these CNPs exhibit unique photoluminescence properties. Interestingly, the CNPs might be exploited to immobilize on the surface of porous silica particles as chromatographic stationary phase. The resultant packing material was evaluated by high-performance liquid chromatography, indicating that the new stationary phase could be used in hydrophilic interaction liquid chromatography (HILIC) and per aqueous liquid chromatography (PALC) modes. The separation of five nucleosides, four sulfa compounds and safflower injection was achieved by using the new column in the HILIC and PALC modes, respectively.

Quantitation of Metformin in Human Plasma and Urine by Hydrophilic Interaction Liquid Chromatography and Application to a Pharmacokinetic Study

DEFF Research Database (Denmark)

Nielsen, Flemming; Hougaard Christensen, Mette Marie; Brøsen, Kim

2014-01-01

: We describe an analytical method for the quantification of the widely used antihyperglycemic agent, metformin, in human plasma and urine. The separation was performed using isocratic hydrophilic interaction liquid chromatography on a Luna hydrophilic interaction liquid chromatography column (125...

Liquid chromatography-tandem mass spectrometric assay for the tyrosine kinase inhibitor afatinib in mouse plasma using salting-out liquid-liquid extraction

NARCIS (Netherlands)

Sparidans, Rolf W; van Hoppe, Stephanie; Rood, Johannes J M; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H

2016-01-01

A quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay for afatinib, an irreversible inhibitor of the ErbB (erythroblastic leukemia viral oncogene homolog) tyrosine kinase family, was developed and validated. Plasma samples were pre-treated using salting-out

Chemometric simultaneous determination of Sofosbuvir and Ledipasvir in pharmaceutical dosage form

Science.gov (United States)

Khalili, Mahsa; Sohrabi, Mahmoud Reza; Mirzabeygi, Vahid; Torabi Ziaratgahi, Nahid

2018-04-01

Partial least squares (PLS), different families of continuous wavelet transform (CWT), and first derivative spectrophotometry (DS) techniques were studied for quantification of Sofosbuvir (SFB) and Ledipasvir (LDV) simultaneously without separation step. The components were dissolved in Acetonitrile and the spectral behaviors were evaluated in the range of 200 to 400 nm. The ultraviolet (UV) absorbance of LDV exhibits no interferences between 300 and 400 nm and it was decided to predict the LDV amount through the classic spectrophotometry (CS) method in this spectral region as well. Data matrix of concentrations and calibrated models were developed, and then by applying a validation set the accuracy and precision of each model were studied. Actual concentrations versus predicted concentrations plotted and good correlation coefficients by each method resulted. Pharmaceutical dosage form was quantified by developed methods and the results were compared with the High Performance Liquid Chromatography (HPLC) reference method. Analysis Of Variance (ANOVA) in 95% confidence level showed no significant differences among methods.

Prostate cell membrane chromatography-liquid chromatography-mass spectrometry for screening of active constituents from Uncaria rhynchophylla.

Science.gov (United States)

He, Jianyu; Han, Shengli; Yang, Fangfang; Zhou, Nan; Wang, Sicen

2013-01-01

Uncaria rhynchophylla is a traditional Chinese medicinal herb used to treat hypertension and convulsive disorders such as epilepsy. Rat prostate cell membrane chromatography combined with liquid chromatography-mass spectrometry (LC-MS) was used to identify active constituents from U. rhynchophylla extracts. Four compounds (corynoxeine, isorhynchophylline, isocorynoxeine and rhynchophylline) were discovered. Competitive binding assay results indicated that the four compounds were in direct competition at a single common binding site and interacted with α1A adrenergic receptors (α1A-AR) in a manner similar to tamsulosin. Affinity constant values of the four compounds binding with α1A-AR were also measured using rat prostate cell membrane chromatography (CMC). Finally, their pharmacodynamic effects were tested on rat caudal arteries. This CMC combined LC-MS system offers a means of drug discovery by screening natural medicinal herbs for new pharmacologically active molecules targeting specific receptors.

Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

NARCIS (Netherlands)

Wils, E.R.J.; Hulst, A.G.

1988-01-01

The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

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

Science.gov (United States)

Pino, Verónica; Afonso, Ana M

2012-02-10

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

An examination of endoparasites and fecal testosterone levels in flying squirrels (Glaucomys spp.) using high performance liquid chromatography-ultra-violet (HPLC-UV).

Science.gov (United States)

Waksmonski, Sarah N; Huffman, Justin M; Mahan, Carolyn G; Steele, Michael A

2017-08-01

The immuno-competence hypothesis proposes that higher levels of testosterone increases the susceptibility to parasitism. Here we examined the testosterone levels in two species of flying squirrels ( Glaucomys ): one known to regularly host a nematode species ( Strongyloides robustus ) without ill effects ( G. volans ) and a closely related species that is considered negatively affected by the parasite. We quantified fecal testosterone levels in northern and southern flying squirrels ( G. sabrinus, G. volans ) with high-performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV), and compared levels to endoparasites detected in individual squirrels. Qualitatively, we found highest levels of testosterone in male northern flying squirrels infected with Strongyloides robustus . This analytical approach represents an alternative and equally reliable method to using enzyme-linked immunosorbent assay (ELISA), for detecting and quantifying fecal testosterone levels.

An examination of endoparasites and fecal testosterone levels in flying squirrels (Glaucomys spp. using high performance liquid chromatography-ultra-violet (HPLC-UV

Directory of Open Access Journals (Sweden)

Sarah N. Waksmonski

2017-08-01

Full Text Available The immuno-competence hypothesis proposes that higher levels of testosterone increases the susceptibility to parasitism. Here we examined the testosterone levels in two species of flying squirrels (Glaucomys: one known to regularly host a nematode species (Strongyloides robustus without ill effects (G. volans and a closely related species that is considered negatively affected by the parasite. We quantified fecal testosterone levels in northern and southern flying squirrels (G. sabrinus, G. volans with high-performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV, and compared levels to endoparasites detected in individual squirrels. Qualitatively, we found highest levels of testosterone in male northern flying squirrels infected with Strongyloides robustus. This analytical approach represents an alternative and equally reliable method to using enzyme-linked immunosorbent assay (ELISA, for detecting and quantifying fecal testosterone levels.

Application of liquid column chromatography to preconcentration, separation and determination of platinum metals

International Nuclear Information System (INIS)

Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

1986-01-01

Separation and determination of platimum metals using the methods of adsorption, ion-pair, ion-exchange, distributing and sieve chromatography are discussed in the review of literature in 1971-1984. Separation and determination of metals as chelates using the method of adsorption and ion-pair chromatograpy are noted to be most perspective directions of developing highly effective liquid chromatography of inorganic systems

Osteoblast cell membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry for screening specific active components from traditional Chinese medicines.

Science.gov (United States)

Wang, Nani; Zhang, Qiaoyan; Xin, Hailiang; Shou, Dan; Qin, Luping

2017-11-01

A method using osteoblast membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry was developed to recognize and identify the specific active components from traditional Chinese medicines. Primary rat osteoblasts were used for the preparation of the stationary phase in the cell chromatography method. Retention components from the cell chromatography were collected and analyzed by liquid chromatography with time-of-flight mass spectrometry. This method was applied in screening active components from extracts of four traditional Chinese medicines. In total, 24 potentially active components with different structures were retained by osteoblast cell chromatography. There were five phenolic glucosides and one triterpenoid saponin from Curculigo orchioides Gaertn, two organic acids and ten flavonoids from Epimedium sagittatum Maxim, one phthalide compound and one organic acid from Angelica sinensis Diels, and two flavonoids and two saponins from Anemarrhena asphodeloides Bunge. Among those, four components (icariin, curculigoside, ferulaic acid, and timosaponin BII) were used for in vitro pharmacodynamics validation. They significantly increased the osteoblast proliferation, alkaline phosphatase activity, levels of bone gla protein and collagen type 1, and promoted mineralized nodule formation. The developed method was an effective screening method for finding active components from complex medicines that act on bone diseases. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Metabolite Extraction from Saccharomyces cerevisiae for Liquid Chromatography-Mass Spectrometry.

Science.gov (United States)

Rosebrock, Adam P; Caudy, Amy A

2017-09-01

Prior to mass spectrometric analysis, cellular small molecules must be extracted and separated from interfering components such as salts and culture medium. To ensure minimal perturbation of metabolism, yeast cells grown in liquid culture are rapidly harvested by filtration as described here. Simultaneous quenching of metabolism and extraction is afforded by immediate immersion in low-temperature organic solvent. Samples prepared using this method are suitable for a range of downstream liquid chromatography-mass spectrometry analyses and are stable in solvent for >1 yr at -80°C. © 2017 Cold Spring Harbor Laboratory Press.

A novel liquid chromatography method using diode-array detector for the determination of oleuropein in dietary supplements.

Science.gov (United States)

Bertolini, Tiziana; Vicentini, Lorenza; Boschetti, Silvia; Andreatta, Paolo; Gatti, Rita

2016-09-10

A simple and fast chromatographic method using ultraviolet diode-array detector (UV-DAD) was developed for the automatic high performance liquid chromatography (HPLC) determination of the title of oleuropein in a new dietary supplements in form of effervescent granules. The chromatographic separations were performed on a C18 core-shell column with detection at λ=232nm. The mobile phase consisted of deionized water with 0.1% TFA and acetonitrile under gradient conditions at a flow-rate of 0.8mL/min. Oleuropein and oleuroside present in the raw material were characterized by high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). The validation of the analytical procedure has been performed determining the following parameters: specificity, linearity, repeatability, reproducibility, accuracy, limit of quantification (LOQ), stability of the standard and sample solutions. Linear response was observed in fortified placebo solutions (determination coefficient: 0.9998). Intra-day precision (relative standard deviation, RSD) was ≤5.0% for peak area and for retention times (tR) without significant differences between intra- and inter-day data. The limits of quantitation (LOQ) was about 5μg/mL and 9pmol/inject. Oleuropein recovery studies gave good results (99.9%) with a R.S.D. of 0.5%. The speed of analysis and the stability of the solutions with a fluctuation Δ (%) ≤2.0 at room temperature means an undoubted advantage of the method allowing the simultaneous preparation of many samples and consecutive chromatographic analyses by using an autosampler. The developed method is suitable for the quality control of oleuropein in raw material and industrial products. The method can be applied in any analytical laboratory not requiring a sophisticated instrumentation. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative analysis of benzodiazepines in vitreous humor by high-performance liquid chromatography

Science.gov (United States)

Bazmi, Elham; Behnoush, Behnam; Akhgari, Maryam; Bahmanabadi, Leila

2016-01-01

Objective: Benzodiazepines are frequently screened drugs in emergency toxicology, drugs of abuse testing, and in forensic cases. As the variations of benzodiazepines concentrations in biological samples during bleeding, postmortem changes, and redistribution could be biasing forensic medicine examinations, hence selecting a suitable sample and a validated accurate method is essential for the quantitative analysis of these main drug categories. The aim of this study was to develop a valid method for the determination of four benzodiazepines (flurazepam, lorazepam, alprazolam, and diazepam) in vitreous humor using liquid–liquid extraction and high-performance liquid chromatography. Methods: Sample preparation was carried out using liquid–liquid extraction with n-hexane: ethyl acetate and subsequent detection by high-performance liquid chromatography method coupled to diode array detector. This method was applied to quantify benzodiazepines in 21 authentic vitreous humor samples. Linear curve for each drug was obtained within the range of 30–3000 ng/mL with coefficient of correlation higher than 0.99. Results: The limit of detection and quantitation were 30 and 100 ng/mL respectively for four drugs. The method showed an appropriate intra- and inter-day precision (coefficient of variation forensic toxicology laboratory. PMID:27635251

Separation of hemagglutination-inhibiting immunoglobulin M antibody to rubella virus in human serum by high-performance liquid chromatography.

OpenAIRE

Kobayashi, N; Suzuki, M; Nakagawa, T; Matumoto, M

1986-01-01

High-performance liquid chromatography was successfully used to separate hemagglutination-inhibiting immunoglobulin M (IgM) rubella virus antibody from IgG rubella virus antibody in human serum. The fractionation by high-performance liquid chromatography was as effective as sucrose density gradient centrifugation in separating IgM antibody from IgG antibody.

Combined high-performance liquid chromatography-radioimmunoassay for cytokinins

International Nuclear Information System (INIS)

MacDonald, E.M.S.; Akiyoshi, D.E.; Morris, R.O.

1981-01-01

The cytokinins isopentenyladenosine and ribosylzeatin were conjugated to bovine serum albumin and the conjugates used to raise antisera in rabbits. The resulting antisera had high specificity towards the cytokinin haptens and low cross-reactivity towards other purines. They were used as the basis for a radioimmunoassay for cytokinins, which, when applied in conjunction with high-performance liquid chromatography, allowed rapid and sensitive (to the picogram range) estimation and identification of multiple cytokinins from natural plant and bacterial sources. (orig.)

Development of a high-performance liquid chromatography method for the determination of florfenicol in animal feedstuffs.

Science.gov (United States)

Yang, JinJing; Sun, GuiZhi; Qian, MingRong; Huang, LingLi; Ke, XianBing; Yang, Bo

2017-11-15

An effective thin layer chromatography (TLC) purification procedure coupled to high-performance liquid chromatography (HPLC) method was developed for the determination of florfenicol (FF) in pig, chicken and fish feedstuffs. The feedstuff samples were extracted with ethyl acetate, defatted with n-hexane saturated with acetonitrile, and further purified by TLC. The chromatographic separation was performed on a Waters Symmetry C 18 column using an isocratic procedure with acetonitrile-water (35:65, v/v) at 0.6mL/min. The ultraviolet (UV) detector was set at a wavelength of 225nm. The FF concentrations in feedstuff samples were quantified using a standard curve. Good linear correlations (y=159075x-15054, r>0.9999) were achieved within the concentration range of 0.05-200μg/mL. The recoveries of FF spiked at levels of 1, 100 and 1000μg/g ranged from 80.6% to 105.3% with the intra-day and inter-day relative standard deviation (RSD) less than 9.3%. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.06mg/kg for pig feedstuffs, 0.02 and 0.07mg/kg for chicken feedstuffs, and 0.02 and 0.05mg/kg for fish feedstuffs, respectively. This reliable, simple and cost-effective method could be applied to the routine monitoring of FF in animal feedstuffs. Copyright © 2017 Elsevier B.V. All rights reserved.

Taste characteristics of Chinese bayberry juice characterized by sensory evaluation, chromatography analysis, and an electronic tongue.

Science.gov (United States)

Yu, Haiyan; Zhang, Yan; Zhao, Jie; Tian, Huaixiang

2018-05-01

To evaluate the taste characteristics of Chinese bayberry juice, four types of bayberry juice sourced from different origins and varieties were analysed using sensory evaluation, chromatography, spectroscopy analysis and an electronic tongue (E-tongue). Nine organic acids and three sugars were assessed using high performance liquid chromatography. Total polyphenols were measured by spectrophotometry. The overall taste profile was collected using the E-tongue. The four types of bayberry juice differed in the sensory attributes of sour, sweet, bitter, and astringent. The E-tongue responses combined with discriminant analysis were able to characterise the taste profiles of the juices. The relationships between the taste compounds and the sensory panel scores established by partial least squares showed that total polyphenols, quininic acid, maleic acid, fructose, citric acid, lactic acid, succinic acid and sucrose made significant contributions to the taste characteristics of the Chinese bayberry juice.

Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

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

2016-04-01

In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simple measurement of isepamicin, a new aminoglycoside antibiotic, in guinea pig and human plasma, using high-performance liquid chromatography with ultraviolet detection

International Nuclear Information System (INIS)

Dionisotti, S.; Bamonte, F.; Scaglione, F.; Ongini, E.

1991-01-01

Isepamicin, the 1-N-(S-alpha-hydroxy-beta-aminopropionyl) derivative of gentamicin B, is a new aminoglycoside antibiotic, which not only has most of the properties of amikacin but also is effective against several amikacin-resistant strains of bacteria. The drug was assayed in guinea-pig and human plasma with a high-performance liquid chromatographic procedure using precolumn derivatization with 1-fluoro-2,4-dinitrobenzene and ultraviolet detection. Linearity was established over the range 0.5-40 micrograms/ml using 50 microliters of plasma. Accuracy has a mean relative error of less than 3% and precision a mean coefficient of variation of 5%. Isepamicin was determined without interference from plasma constituents or other drugs commonly prescribed during aminoglycoside therapy. This procedure correlates well with radioimmunoassay and can be used either in experimental studies or therapeutic monitoring of plasma levels

Liquid to liquid extraction and liquid chromatography-tandem mass spectrometry determination of hainanmycin in feed.

Science.gov (United States)

Wang, Ze Ping; Shen, Jian Zhong; Linhardt, Robert J; Jiang, Hui; Cheng, Lin Li

2017-03-01

Hainanmycin is a new veterinary polyether antibiotic and has few sensitive analytical method in present days. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) relying on multiple reaction monitoring (MRM) detection was developed for analysis of hainanmycin in animal feed. Feed samples were extracted with ethyl acetate and purified by two steps of liquid-liquid extraction (LLE) to get rid of water solvable matrix and lipids one by one. The final simple was analyzed by LC-MS/MS. The LC mobile phase was composed of 0.1% aqueous formic acid and 0.1% formic acidified acetonitrile by gradient elution. Average recoveries ranged from 74.22% to 87.85%, as determined by spiking with 2.0 (LOQ) ∼2500μgkg -1 of hainanmycin. The inter-day and intra-day coefficient of variation was 9.21% to 11.77% and 7.67% to 13.49%, respectively. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.36μgkg -1 and 2.0μgkg -1 , respectively. Copyright © 2016. Published by Elsevier B.V.

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

Science.gov (United States)

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

2016-05-01

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

Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

Science.gov (United States)

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-01-01

A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

High-Performance Liquid Chromatographic Ultraviolet Determination of Memantine Hydrochloride after In Vitro Transdermal Diffusion Studies

Directory of Open Access Journals (Sweden)

Sergio del Rio-Sancho

2013-01-01

Full Text Available The purpose of the present work was to validate an accurate and precise high-performance liquid chromatography (HPLC method involving ultraviolet detection for the quantitative analysis of memantine hydrochloride. In order to analyze a molecule with no chromophoric groups that could be detected by a UV/visible detector, it was necessary to extract the drug and to perform a dansylation reaction that enabled the UV/visible detection of the derivatized molecule. Separation was carried out with a 150 mm Kromasil C18 column at room temperature. The detection response, at 218 nm, was found to be linear in the concentration range from 0.5 to 50 μg/mL. The method was validated for specificity, linearity, precision, accuracy, limit of detection, limit of quantification, and robustness. The limit of detection (LOD was 0.144 μg/mL, and the limit of quantification (LOQ was 0.437 μg/mL. The dansylated memantine complex was stable for at least five days in all the conditions evaluated. The potential use of this method has been demonstrated by the quantification of memantine hydrochloride contained in samples from the study of its in vitro transdermal permeation.

Quantitative analysis of phylloquinone (vitamin K1) in soy bean oils by high-performance liquid chromatography.

Science.gov (United States)

Zonta, F; Stancher, B

1985-07-19

A high-performance liquid chromatographic method for determining phylloquinone (vitamin K1) in soy bean oils is described. Resolution of vitamin K1 from interfering peaks of the matrix was obtained after enzymatic digestion, extraction and liquid-solid chromatography on alumina. An isocratic reversed-phase chromatography with UV detection was used in the final stage. The quantitation was carried out by the standard addition method, and the recovery of the whole procedure was 88.2%.

Identification and Quantification of the Major Constituents in Egyptian Carob Extract by Liquid Chromatography?Electrospray Ionization-Tandem Mass Spectrometry

OpenAIRE

Owis, Asmaa Ibrahim; El-Naggar, El-Motaz Bellah

2016-01-01

Background: Carob - Ceratonia siliqua L., commonly known as St John's-bread or locust bean, family Fabaceae - is one of the most useful native Mediterranean trees. There is no data about the chromatography methods performed by high performance liquid chromatography (HPLC) for determining polyphenols in Egyptian carob pods. Objective: To establish a sensitive and specific liquid chromatography?electrospray ionization (ESI)-tandem mass spectrometry (MSn) methodology for the identification of th...

Glucose and glycerol concentrations and their tracer enrichment measurements using liquid chromatography tandem mass spectrometry

DEFF Research Database (Denmark)

Bornø, Andreas; Foged, Lene; van Hall, Gerrit

2014-01-01

The present study describes a new liquid chromatography tandem mass spectrometry method for high-throughput quantification of glucose and glycerol in human plasma using stable isotopically labeled internal standards and is suitable for simultaneous measurements of glucose and glycerol enrichments...... of variation were 2.0% and 9.7%, respectively. After derivatization, plasma samples were stable for at least 14 days. In conclusion, we have developed and validated a novel, accurate, and sensitive high-throughput liquid chromatography tandem mass spectrometry method for simultaneous determination of glucose...

Determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry

Science.gov (United States)

Hostetler, K.A.; Thurman, E.M.

2000-01-01

Analytical methods using high-performance liquid chromatography-diode array detection (HPLC-DAD) and high-performance liquid chromatography/mass spectrometry (HPLC/MS) were developed for the analysis of the following chloroacetanilide herbicide metabolites in water: alachlor ethanesulfonic acid (ESA); alachlor oxanilic acid; acetochlor ESA; acetochlor oxanilic acid; metolachlor ESA; and metolachlor oxanilic acid. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The average HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.5 and 2.0 ??g/l ranged from 84 to 112%, with relative standard deviations of 18% or less. The average HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.2 and 2.0 ??g/l ranged from 81 to 118%, with relative standard deviations of 20% or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 ??g/l, whereas the LOQ using the HPLC/MS method was at 0.05 ??g/l. These metabolite-determination methods are valuable for acquiring information about water quality and the fate and transport of the parent chloroacetanilide herbicides in water. Copyright (C) 2000 Elsevier Science B.V.

Deformation and degradation of polymers in ultra-high-pressure liquid chromatography

NARCIS (Netherlands)

Uliyanchenko, E.; van der Wal, S.; Schoenmakers, P.J.

2011-01-01

Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles

Core-shell microspheres with porous nanostructured shells for liquid chromatography.

Science.gov (United States)

Ahmed, Adham; Skinley, Kevin; Herodotou, Stephanie; Zhang, Haifei

2018-01-01

The development of new stationary phases has been the key aspect for fast and efficient high-performance liquid chromatography separation with relatively low backpressure. Core-shell particles, with a solid core and porous shell, have been extensively investigated and commercially manufactured in the last decade. The excellent performance of core-shell particles columns has been recorded for a wide range of analytes, covering small and large molecules, neutral and ionic (acidic and basic), biomolecules and metabolites. In this review, we first introduce the advance and advantages of core-shell particles (or more widely known as superficially porous particles) against non-porous particles and fully porous particles. This is followed by the detailed description of various methods used to fabricate core-shell particles. We then discuss the applications of common silica core-shell particles (mostly commercially manufactured), spheres-on-sphere particles and core-shell particles with a non-silica shell. This review concludes with a summary and perspective on the development of stationary phase materials for high-performance liquid chromatography applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Coupling nanoliter high-performance liquid chromatography to inductively coupled plasma mass spectrometry for arsenic speciation.

Science.gov (United States)

Cheng, Heyong; Shen, Lihuan; Liu, Jinhua; Xu, Zigang; Wang, Yuanchao

2018-04-01

Nanoliter high-performance liquid chromatography shows low consumption of solvents and samples, offering one of the best choices for arsenic speciation in precious samples in combination with inuctively coupled plasma mass spectrometry. A systematic investigation on coupling nanoliter high-performance liquid chromatography to inductively coupled plasma mass spectrometry from instrument design to injected sample volume and mobile phase was performed in this study. Nanoflow mobile phase was delivered by flow splitting using a conventional high-pressure pump with reuse of mobile phase waste. Dead volume was minimized to 60 nL for the sheathless interface based on the previously developed nanonebulizer. Capillary columns for nanoliter high-performance liquid chromatography were found to be sensitive to sample loading volume. An apparent difference was also found between the mobile phases for nanoliter and conventional high-performance liquid chromatography. Baseline separation of arsenite, arsenate, monomethylarsenic, and dimethylarsenic was achieved within 11 min on a 15 cm C 18 capillary column and within 12 min on a 25 cm strong anion exchange column. Detection limits of 0.9-1.8 μg/L were obtained with precisions variable in the range of 1.6-4.2%. A good agreement between determined and certified values of a certified reference material of human urine (GBW 09115) validated its accuracy along with good recoveries (87-102%). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

Science.gov (United States)

Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

2015-03-27

A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

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

DEFF Research Database (Denmark)

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

2008-01-01

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

Simultaneous high-performance liquid chromatographic determination of nitrate, nitrite, and organic pesticides in soil solution using a multidimensional column with ultraviolet detection

International Nuclear Information System (INIS)

Nkedi-Kizza, P.; Owusu-Yaw, J.

1992-01-01

In many fertilizer trials, the amount of nitrate-nitrogen in soil solution must be quantified frequently because nitrate is easily leached. Because pesticides are generally applied to cropland with fertilizers, quantitative information is needed on the concentration of these chemicals still available in the soil. Information on nitrite, nitrate and pesticide concentrations in food, water and environmental samples is essential because of their toxicity and potential for groundwater and surface water contamination. Most of the methods currently used for nitrate determination also account for nitrite, because nitrite and some organics act as interferences. Some of the existing analytical methods require sample reduction or derivatization, complex solvent mixtures or large sample volumes which make analysis times long. A High-Performance Liquid Chromatography (HPLC) method has been developed for the simultaneous determination of nitrate, nitrite and organic pesticides in soil solution samples and extracts using a multidimensional separator column with ultraviolet detection at 220 nm. The method is rapid and requires small sample volumes (20 μL). It is a sensitive method which is suitable for routine analyses of up to 100 samples per day. A comparison of this method with standard ion chromatography with conductivity detection showed very good agreement between the two methods for the analysis of NO3- and NO2-

Liquid chromatography tandem mass spectrometry determination of total budesonide levels in dog plasma after inhalation exposure.

Science.gov (United States)

Berg, Seija; Melamies, Marika; Rajamäki, Minna; Vainio, Outi; Peltonen, Kimmo

2012-01-01

A sensitive and selective method to quantify budesonide in dog plasma samples was developed and fully validated. Liquid-liquid extraction was followed by solid-phase extraction and liquid chromatography-tandem mass spectrometry with electrospray ionization. After reconstitution of the analytes in the mobile phase, samples were analysed by reversed-phase liquid chromatography with isocratic elution. d8-Budesonide was used as an internal standard, and characteristic transitions of d8-budesonide and budesonide were used for quantification. The method was validated with respect to selectivity, specificity, linearity, recovery, repeatability, reproducibility and limits of detection and quantification. The validated method was successfully applied to monitor the plasma levels of budesonide in dogs exposed to clinical doses of inhaled and intravenous drug.

Atomic absorption spectrophotometry in perspective

International Nuclear Information System (INIS)

Soffiantini, V.

1981-01-01

Atomic absorption spectrophotometry is essentially an analytical technique used for quantitative trace metal analysis in a variety of materials. The speed and specificity of the technique is its greatest advantage over other analytical techniques. What atomic absorption spectrophotometry can and cannot do and its advantages and disadvantages are discussed, a summary of operating instructions are given, as well as a summary of analytical interferences. The applications of atomic absorption spectrophotometry are also shortly discussed

Lead Quantification in Urine Samples of Athletes by Coupling DLLME with UV-Vis Spectrophotometry.

Science.gov (United States)

Faraji, Hakim; Helalizadeh, Masoumeh

2017-04-01

Urine lead level is one of the most employed measures of lead exposure and risk. The urine samples used in this study were obtained from ten healthy male cyclists. Dispersive liquid-liquid microextraction combined with ultraviolet and visible spectrophotometry was utilized for preconcentration, extraction, and determination of lead in urine samples. Optimization of the independent variables was carried out based on chemometric methods in three steps. According to the screening and optimization study, 133 μL of CCl 4 (extracting solvent), 1.34 mL ethanol (dispersing solvent), pH 2.0, 0.00 % of salt, and 0.1 % O,O-diethyl dithiophosphoric (chelating agent) were used as the optimum independent variables for microextraction and determination of lead. Under the optimized conditions, R 2 was 0.9991, and linearity range was 0.01-100 μg L -1 . Precision was evaluated in terms of repeatability and intermediate precision, with relative standard deviations being <9.1 and <15.3 %, respectively. The accuracy was estimated using urine samples of cyclists as real samples and it was confirmed. The relative error of ≤5 % was considered significant in the method specificity study. The lead concentration mean for the cyclists was 3.79 μg L -1 in urine samples. As a result, the proposed method is a robust technique to quantify lead concentrations higher than 11.6 ng L -1 in urine samples.

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

Science.gov (United States)

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

2016-07-01

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

Assessing the detectability of antioxidants in two-dimensional high-performance liquid chromatography.

Science.gov (United States)

Bassanese, Danielle N; Conlan, Xavier A; Barnett, Neil W; Stevenson, Paul G

2015-05-01

This paper explores the analytical figures of merit of two-dimensional high-performance liquid chromatography for the separation of antioxidant standards. The cumulative two-dimensional high-performance liquid chromatography peak area was calculated for 11 antioxidants by two different methods--the areas reported by the control software and by fitting the data with a Gaussian model; these methods were evaluated for precision and sensitivity. Both methods demonstrated excellent precision in regards to retention time in the second dimension (%RSD below 1.16%) and cumulative second dimension peak area (%RSD below 3.73% from the instrument software and 5.87% for the Gaussian method). Combining areas reported by the high-performance liquid chromatographic control software displayed superior limits of detection, in the order of 1 × 10(-6) M, almost an order of magnitude lower than the Gaussian method for some analytes. The introduction of the countergradient eliminated the strong solvent mismatch between dimensions, leading to a much improved peak shape and better detection limits for quantification. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High performance liquid chromatography in studies of radiolabeled antibodies

International Nuclear Information System (INIS)

Hnatowich, D.J.

1986-01-01

High performance liquid chromatography (HPLC) as applied to the separation of antibodies displays the same advantages as in its other applications, namely good resolution accompanied by fast analysis. It is therefore not surprising that many HPLC columns designed for use with antibodies and other proteins are now available commercially. The properties of proteins which provide the separation are size, hydrophobicity, charge and affinity. The features of each are discussed. (author)

Rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Yang, Xiao; Diao, Chun-Peng; Sun, Ai-Ling; Liu, Ren-Min

2014-10-01

A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut-glass dropper was designed and applied to collect the floating extraction drop in liquid-liquid microextraction when low-density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low-density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex-assisted liquid-liquid microextraction was employed to investigate the usefulness of the apparatus. High-performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r(2) = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Deformation and degradation of polymers in ultra-high-pressure liquid chromatography.

Science.gov (United States)

Uliyanchenko, Elena; van der Wal, Sjoerd; Schoenmakers, Peter J

2011-09-28

Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles and narrow bore tubing in combination with high pressures generate significant shear and extensional forces in UHPLC systems, which may affect polymer chains. At high stress conditions flexible macromolecules may become extended and eventually the chemical bonds in the molecules can break. Deformation and degradation of macromolecules will affect the peak retention and the peak shape in the chromatogram, which may cause errors in the obtained results (e.g. the calculated molecular-weight distributions). In the present work we explored the limitations of UHPLC for the analysis of polymers. Degradation and deformation of macromolecules were studied by collecting and re-injecting polymer peaks and by off-line two-dimensional liquid chromatography. Polystyrene standards with molecular weight of 4 MDa and larger were found to degrade at UHPLC conditions. However, for most polymers degradation could be avoided by using low linear velocities. No degradation of 3-MDa PS (and smaller) was observed at linear velocities up to 7 mm/s. The column frits were implicated as the main sources of polymer degradation. The extent of degradation was found to depend on the type of the column and on the column history. At high flow rates degradation was observed without a column being installed. We demonstrated that polymer deformation preceded degradation. Stretched polymers eluted from the column in slalom chromatography mode (elution order opposite to that in SEC or HDC). Under certain conditions we observed co-elution of large and small PS molecules though a convolution of slalom chromatography and hydrodynamic chromatography. Copyright © 2011 Elsevier B.V. All rights reserved.

Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

Science.gov (United States)

Baghdady, Yehia Z; Schug, Kevin A

2016-01-01

Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multi-detection of corticosteroids in sports doping and veterinary control using high-resolution liquid chromatography/time-of-flight mass spectrometry

NARCIS (Netherlands)

Touber, M.E.; Engelen, M.C.; Georgakopoulus, C.; Rhijn, van J.A.; Nielen, M.W.F.

2007-01-01

A liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) method was developed using the latest high-resolution LC column technology, the ultra performance liquid chromatography (UPLC (TM)), and electrospray ionization (ESI) in the positive ion mode. Gradient UPLC separation conditions

Degradation of surface-active compounds in a constructed wetland determined using high performance liquid chromatography and extraction spectrophotometry

Czech Academy of Sciences Publication Activity Database

Sima, J.; Pazderník, M.; Tříska, Jan; Svoboda, L.

2013-01-01

Roč. 48, č. 5 (2013), s. 559-567 ISSN 1093-4529 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0073 Institutional support: RVO:67179843 Keywords : Municipal wastewater * organic pollutants * anionic and nonionic surfactants * seasonal monitoring * reed bed * ion pair chromatography * environmental analytical chemistry Subject RIV: EH - Ecology, Behaviour Impact factor: 1.135, year: 2013

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

Science.gov (United States)

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

2018-03-30

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

Current practice of liquid chromatography-mass spectrometry in metabolomics and metabonomics.

Science.gov (United States)

Gika, Helen G; Theodoridis, Georgios A; Plumb, Robert S; Wilson, Ian D

2014-01-01

Based on publication and citation numbers liquid chromatography (LC-MS) has become the major analytical technology in the field of global metabolite profiling. This dominance reflects significant investments from both the research community and instrument manufacturers. Here an overview of the approaches taken for LC-MS-based metabolomics research is given, describing critical steps in the realisation of such studies: study design and its needs, specific technological problems to be addressed and major obstacles in data treatment and biomarker identification. The current state of the art for LC-MS-based analysis in metabonomics/metabolomics is described including recent developments in liquid chromatography, mass spectrometry and data treatment as these are applied in metabolomics underlining the challenges, limitations and prospects for metabolomics research. Examples of the application of metabolite profiling in the life sciences focusing on disease biomarker discovery are highlighted. In addition, new developments and future prospects are described. Copyright © 2013 Elsevier B.V. All rights reserved.

The gas–liquid chromatography of carboxylic acid esters of the urinary 11-deoxy-17-oxo steroids

Science.gov (United States)

Sadler, Patricia A.; Kellie, A. E.

1967-01-01

1. The gas–liquid-chromatographic separations of the acetate, propionate, n-butyrate, isobutyrate and n-valerate esters of androsterone, aetiocholanolone and dehydroepiandrosterone were studied on a 1% neopentyl glycol sebacate column. The n-butyrate, isobutyrate and n-valerate esters were well resolved. 2. The three steroids derived from hydrolysed urinary 17-oxo steroid conjugate extracts were analysed by gas–liquid chromatography after conversion into their n-butyrate esters. The results were compared with independent determinations involving chromatography on alumina. PMID:4227802

Sensitive quantification of coixol, a potent insulin secretagogue, in Scoparia dulcis extract using high-performance liquid chromatography combined with tandem mass spectrometry and UV detection.

Science.gov (United States)

Ali, Arslan; Haq, Faraz Ul; Ul Arfeen, Qamar; Sharma, Khaga Raj; Adhikari, Achyut; Musharraf, Syed Ghulam

2017-10-01

Diabetes is a major global health problem which requires new studies for its prevention and control. Scoparia dulcis, a herbal product, is widely used for treatment of diabetes. Recent studies demonstrate coixol as a potent and nontoxic insulin secretagog from S. dulcis. This study focuses on developing two quantitative methods of coixol in S. dulcis methanol-based extracts. Quantification of coixol was performed using high-performance liquid chromatography-tandem mass spectrometry (method 1) and high-performance liquid chromatography-ultraviolet detection (method 2) with limits of detection of 0.26 and 11.6 pg/μL, respectively, and limits of quantification of 0.78 and 35.5 pg/μL, respectively. S. dulcis is rich in coixol content with values of 255.5 ± 2.1 mg/kg (method 1) and 220.4 ± 2.9 mg/kg (method 2). Excellent linearity with determination coefficients >0.999 was achieved for calibration curves from 10 to 7500 ng/mL (method 1) and from 175 to 7500 ng/mL (method 2). Good accuracy (bias < -8.6%) and precision (RSD < 8.5%) were obtained for both methods. Thus, they can be employed to analyze coixol in plant extracts and herbal formulations. Copyright © 2017 John Wiley & Sons, Ltd.

Identification, characterization, and high-performance liquid chromatography quantification of process-related impurities in vonoprazan fumarate.

Science.gov (United States)

Liu, Lei; Cao, Na; Ma, Xingling; Xiong, Kaihe; Sun, Lili; Zou, Qiaogen

2016-04-01

High-performance liquid chromatography analysis of vonoprazan fumarate, a novel proton pump inhibitor drug revealed six impurities. These were identified by liquid chromatography with mass spectrometry. Further, the structures of the impurities were confirmed by synthesis followed by characterization by mass spectrometry, NMR spectroscopy, and infrared spectroscopy. On the basis of these data and knowledge of the synthetic scheme of vonoprazan fumarate, the previously unknown impurity was identified as 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3-yl]-N-methyldimethylamine, which is a new compound. The possible mechanisms by which these impurities were formed were also discussed. A high-performance liquid chromatography method was optimized in order to separate, selectively detect, and quantify all process-related impurities of vonoprazan fumarate. The presented method has been validated in terms of linearity, limits of detection, and quantification, and response factors and, therefore, is highly suitable for routine analysis of vonoprazan fumarate related substances as well as stability studies. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of goat colostrum oligosaccharides by nano-liquid chromatography on chip quadrupole time-of-flight mass spectrometry and hydrophilic interaction liquid chromatography-quadrupole mass spectrometry.

Science.gov (United States)

Martín-Ortiz, A; Salcedo, J; Barile, D; Bunyatratchata, A; Moreno, F J; Martin-García, I; Clemente, A; Sanz, M L; Ruiz-Matute, A I

2016-01-08

A detailed qualitative and quantitative characterization of goat colostrum oligosaccharides (GCO) has been carried out for the first time. Defatted and deproteinized colostrum samples, previously treated by size exclusion chromatography (SEC) to remove lactose, were analyzed by nanoflow liquid chromatography-quadrupole-time of flight mass spectrometry (Nano-LC-Chip-Q-TOF MS). Up to 78 oligosaccharides containing hexose, hexosamine, fucose, N-acetylneuraminic acid or N-glycolylneuraminic acid monomeric units were identified in the samples, some of them detected for the first time in goat colostra. As a second step, a hydrophilic interaction liquid chromatography coupled to mass spectrometry (HILIC-MS) methodology was developed for the separation and quantitation of the main GCO, both acidic and neutral carbohydrates. Among other experimental chromatographic conditions, mobile phase additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry of target carbohydrates. Narrow peaks (wh: 0.2-0.6min) and good symmetry (As: 0.8-1.4) were obtained for GCO using an acetonitrile:water gradient with 0.1% ammonium hydroxide at 40°C. These conditions were selected to quantify the main oligosaccharides in goat colostrum samples. Values ranging from 140 to 315mgL(-1) for neutral oligosaccharides and from 83 to 251mgL(-1) for acidic oligosaccharides were found. The combination of both techniques resulted to be useful to achieve a comprehensive characterization of GCO. Copyright © 2015 Elsevier B.V. All rights reserved.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

Science.gov (United States)

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

Science.gov (United States)

Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

2016-12-01

Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL -1 , respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultraviolet curing of acrylated liquid natural rubber for surface coating application

Directory of Open Access Journals (Sweden)

Kannikar Kwanming

2009-01-01

Full Text Available Ultraviolet curable acrylated liquid natural rubber was prepared by grafting of photosensitive molecule onto liquid natural rubber for surface coating application. The liquid natural rubber (LNR was firstly obtained by degradation of natural rubber latex with hydrogen peroxide and cobalt acetylacetonate at 65oC for 72 hrs. The preparation of acrylated natural rubber was carried out by the reaction of acrylic acid and epoxidized liquid natural rubber (ELNR prior obtained from LNR with formic acid and hydrogen peroxide in the ratio of 2:1 by weight in toluene at 80oC for 6, 9, 12, 18, and 24 hrs. It was found that the percentage of acrylate grafted onto liquid natural rubber depended on the reaction time. Surface coating was performed by using acrylated liquid natural rubber and 1,6-hexanediol diacrylate (HDDA or tripropylene glycol diacrylate (TPGDA as a crosslinker and Irgarcure 184 or Irgarcure 651 as a photoinitiator under UV exposure for 30, 60, and 90 seconds. The hardness test of cured products was investigated using the Pencil hardness test at pencil level of 2B to 6H. It was found that the highest hardness of surface coating was at pencil level of 4H for the product using TPGDA and Irgacure 651 in the ratio of 80:10 parts per hundred of rubber (phr. The cured products were able to resist to 2% H2SO4 and distilled water for more than 24 hrs.

An Advanced, Interactive, High-Performance Liquid Chromatography Simulator and Instructor Resources

Science.gov (United States)

Boswell, Paul G.; Stoll, Dwight R.; Carr, Peter W.; Nagel, Megan L.; Vitha, Mark F.; Mabbott, Gary A.

2013-01-01

High-performance liquid chromatography (HPLC) simulation software has long been recognized as an effective educational tool, yet many of the existing HPLC simulators are either too expensive, outdated, or lack many important features necessary to make them widely useful for educational purposes. Here, a free, open-source HPLC simulator is…

Determination of veterinary antibiotic residues in foods of animal origin by liquid chromatography

Directory of Open Access Journals (Sweden)

Pedro Enrique La Rosa Zambrano

2018-05-01

Full Text Available TITLE: Determination of veterinary antibiotic residues in foods of animal origin by liquid chromatography Introduction: The presence of certain infectious agents makes necessary the use of antibiotics to ensure the welfare of animals destined for human consumption; however, the withdrawal time must be considered and respected since there is the possibility of finding residues above the permitted levels, which could constitute a risk to public health. Objective: Present a collection of information based on how is performed the detection and quantification of antibiotic residues in various products of animal origin using chromatography methods. Method: Review of databases in Elsevier, SciELO, Springer, Hindawi, FAO, EFSA, Senasa and Sanipes, using keywords such as “liquid chromatography”, “mass spectrometry”, “antibiotic residues” and “products of animal origin” in Spanish and English. Results: They were selected 71 references among articles, book chapters, norms and regulations published between 2000 and 2017, which it is emphasized that chromatographic methodologies for antibiotic residues monitoring must be sensitive, reproducible, reliable and identify volumes in mg/kg; likewise, they must follow the requirements of international standards for the maximum residue limits detecction. Conclusions: Liquid chromatography coupled to a mass spectrometer is the most used technique to allow the separation of complex matrices based on the molecular weight of the compound (antibiotic or its fragments; however, It is complex, expensive and requires highly trained personnel.

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

Science.gov (United States)

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

2013-01-01

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

High performance liquid chromatographic determination of Ginseng saponin by ultraviolet derivatisation

International Nuclear Information System (INIS)

Besso, H.; Saruwatari, Y.; Futamura, K.; Kunihiro, K.; Fuwa, T.; Tanaka, O.

1979-01-01

Ginsenoides Rb 1 , b 2 , c, d, e and g 1 quantitatively reacted with benzoyl chloride in pyridine to afford the respective derivatives having strong UV absorption. The UV-derivatized saponins were separated by high performance liquid chromatography (HPLC), and the saponin-contents of the various Ginseng varieties were determined. It is possible to distinguish white Ginseng from the root hairs of Ginseng by the pattern analysis of HPLC. (orig.) [de

An efficient hydrophilic interaction liquid chromatography separation of 7 phospholipid classes based on a diol column

NARCIS (Netherlands)

Zhu, C.; Dane, A.; Spijksma, G.; Wang, M.; Greef, J. van der; Luo, G.; Hankemeier, T.; Vreeken, R.J.

2012-01-01

A hydrophilic interaction liquid chromatography (HILIC) - ion trap mass spectrometry method was developed for separation of a wide range of phospholipids. A diol column which is often used with normal phase chromatography was adapted to separate different phospholipid classes in HILIC mode using a

Determination of chlorophenols in honey samples using in-situ ionic liquid-dispersive liquid-liquid microextraction as a pretreatment method followed by high-performance liquid chromatography.

Science.gov (United States)

Fan, Chen; Li, Nai; Cao, Xueli

2015-05-01

In-situ ionic liquid-dispersive liquid-liquid microextraction (IL-DLLME) method was developed as a pretreatment method for the detection of six chlorophenols (CPs) in honey samples. The hydrophobic ionic liquid [C4MIM][NTf2], formed in-situ by the hydrophilic ionic liquid [C4MIM][BF4] and the ion exchange reagent LiNTf2 was used as the microextractant solvent of CPs from honey sample. Then the enriched analytes were back-extracted into 40 μL of 0.14 M NaOH solution and finally subjected to analysis by high-performance liquid chromatography. The method showed low limit of detection of CPs, 0.8-3.2 μg/L and high enrichment factor, 34-65 with the recoveries range from 91.60% to 114.33%. The method is simple, rapid, environmentally friendly and with high extraction efficiency. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

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

Directory of Open Access Journals (Sweden)

Senthamil Selvan Perumal

2014-12-01

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

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

Science.gov (United States)

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

2014-12-01

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

Determination of ribavirin in human serum using liquid chromatography tandem mass spectrometry

NARCIS (Netherlands)

van der Lijke, H.; Alffenaar, J.-W. C.; Kok, W.Th.; Greijdanus, B.; Uges, D.R.A.

2012-01-01

A method has been developed for the determination of ribavirin in human serum for therapeutic drug monitoring purposes, using liquid chromatography electrospray ionization mass spectrometry. Separation was obtained with a mobile phase gradient starting and ending in 100% aqueous conditions using a

Study of high performance liquid chromatography fingerprint for traditional chinese medicine yigongningxue oral liquid

International Nuclear Information System (INIS)

Feng, C.; Ruan, J.L.

2010-01-01

A simple, reliable and accurate fingerprinting method has been developed for quality control of YiGongNingXue oral liquid. The separation was done by reverse phase chromatography using Zorbax eclipse XDB C/sub 18/ column (250mmx4.6mmi. d. with 5.0 micro m particle size) and detection at 246nm. Methanol (5-95 % in 70 min)-buffer solution (water-phosphorica cid, pH 3.0, 95-0 percent in 70 min) as mobile phase for linear gradient elution. The flow rate was 1.0 mLmin/sup 1/ and the column temperature was at 25 deg. C. The similarity of 20 batches of YGNX oral liquid was more than 90 %. Also 15 common peaks of chromatogram have been detected, ten of them were identified by comparing fingerprint chromatogram with reference substances The HPLC fingerprint can be used to control the quality of YiGongNingXue oral liquid. (author)

Determination of pertechnetate by liquid chromatography with reductive electrochemical detection

International Nuclear Information System (INIS)

Lewis, J.Y.; Zodda, J.P.; Deutsch, E.; Heineman, W.R.

1983-01-01

A method utilizing liquid chromatography with electrochemical detection has been developed for the determination of total TcO 4 - (/sup 99m/TcO 4 - and /sup 99m/TcO 4 - ) in 99 Mo//sup 99m/Tc generator eluents. Pertechnetate, which is the starting material for the preparation of many diagnostic radiopharmaceuticals, is generally present in these eluents in the concentration range of 5 X 10 -8 M to 5 X 10 -6 M. No sample pretreatment is necessary since impurities and other components are separated by the high-pressure liquid chromatography (HPLC) NH 2 -bonded column. By use of both static mercury drop (SMDE) and solid electrode detectors, in conjuction with rigorous deoxygenation procedures, total TcO 4 - in generator eluents is readily determined. A severe electrode fouling phenomenon limits the use of solid electrode detectors to TcO 4 - concentrations less than 10 -7 M, the working range for a carbon electrode being 8.5 X 10 -9 to 1.0 X 10 -7 M. The working range for the SMDE is 2.1 X 10 -8 to 1.0 X 10 -4 M TcO 4 -

Molecular differences between deuterated and protonated polystyrenes using reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Kayillo, Sindy; Gray, Michael J; Shalliker, R Andrew; Dennis, Gary R

2005-05-06

Isotopic substitution is a technique used to highlight particular bonds within a molecule for kinetic, spectroscopic and structure analysis. It is presumed that although some properties such as stretching frequencies will not be the same for substituted analogues, the chemical interactions will not vary appreciably as a function of labelling. Reversed-phase liquid chromatography has been used to demonstrate that there are significant differences between the chromatographic behaviour of a sequence of deuterated and protonated oligomeric polystyrenes. Two-dimensional reversed-phase liquid chromatography was used to show that even the diasteromers of the oligomers (n = 5) have retention mechanisms that are dependent on the subtle changes to the molecular conformation and electronic structure, which are a consequence of deuteration.

Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

Science.gov (United States)

Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

2017-07-01

A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

NARCIS (Netherlands)

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

1995-01-01

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

Analysis of new psychoactive substances in human urine by ultra-high performance supercritical fluid and liquid chromatography: Validation and comparison.

Science.gov (United States)

Borovcová, Lucie; Pauk, Volodymyr; Lemr, Karel

2018-05-01

New psychoactive substances represent serious social and health problem as tens of new compounds are detected in Europe annually. They often show structural proximity or even isomerism, which complicates their analysis. Two methods based on ultra high performance supercritical fluid chromatography and ultra high performance liquid chromatography with mass spectrometric detection were validated and compared. A simple dilute-filter-and-shoot protocol utilizing propan-2-ol or methanol for supercritical fluid or liquid chromatography, respectively, was proposed to detect and quantify 15 cathinones and phenethylamines in human urine. Both methods offered fast separation (chromatography. Limits of detection in urine ranged from 0.01 to 2.3 ng/mL, except for cathinone (5 ng/mL) in supercritical fluid chromatography. Nevertheless, this technique distinguished all analytes including four pairs of isomers, while liquid chromatography was unable to resolve fluoromethcathinone regioisomers. Concerning matrix effects and recoveries, supercritical fluid chromatography produced more uniform results for different compounds and at different concentration levels. This work demonstrates the performance and reliability of supercritical fluid chromatography and corroborates its applicability as an alternative tool for analysis of new psychoactive substances in biological matrixes. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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

2018-01-01

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

Liquid Chromatography for Analysis of Metformin in Myrmeleon sp.

OpenAIRE

Afidatul Muadifah; Hermin Sulistyarti; Sasangka Prasetyawan

2017-01-01

Myrmeleon sp is a typical of insect larva which has been used in Indonesia for diabetes treatment. However, there is no sufficient scientific report explaining the bioactive compounds in this insect. Based on our preliminary research, this insect contained metformin, i.e. one of bioactive compounds for the treatment of type-2 diabetes. Therefore, this study is focused on the development of separation technique using high performance liquid chromatography (HPLC) on a reverse phase C-18 column ...

Preparation and Characterization of a Polymeric Monolithic Column for Use in High-Performance Liquid Chromatography (HPLC)

Science.gov (United States)

Bindis, Michael P.; Bretz, Stacey Lowery; Danielson, Neil D.

2011-01-01

The high-performance liquid chromatography (HPLC) experiment, most often done in the undergraduate analytical instrumentation laboratory course, generally illustrates reversed-phase chromatography using a commercial C[subscript]18 silica column. To avoid the expense of periodic column replacement and introduce a choice of columns with different…

Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection.

Science.gov (United States)

Fan, Wenying; He, Man; You, Linna; Zhu, Xuewei; Chen, Beibei; Hu, Bin

2016-04-22

Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37 μg L(-1), and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5 μg L(-1) and the relative standard deviation (RSD) was found to be 7.3% (n=7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine

Separation and quantification of ropinirole and some impurities using capillary liquid chromatography

NARCIS (Netherlands)

Coufal, P.; Stulik, K.; Claessens, H.A.; Hardy, M.J.; Webb, M.

1999-01-01

Ropinirole, 4-[2-(dipropylamino)ethyl]-1,3-dihydro-2H-indol-2-one, is a potent anti-Parkinson’s disease drug developed by SmithKline Beecham Pharmaceuticals. Capillary liquid chromatography (CLC) was used for the separation and quantification of ropinirole and its five related impurities,

Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

Science.gov (United States)

You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

2018-01-15

A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

Detection of Stimulants and Narcotics by Liquid Chromatography-Tandem Mass Spectrometry and Gas Chromatography-Mass Spectrometry for Sports Doping Control.

Science.gov (United States)

Ahrens, Brian D; Kucherova, Yulia; Butch, Anthony W

2016-01-01

Sports drug testing laboratories are required to detect several classes of compounds that are prohibited at all times, which include anabolic agents, peptide hormones, growth factors, beta-2 agonists, hormones and metabolic modulators, and diuretics/masking agents. Other classes of compounds such as stimulants, narcotics, cannabinoids, and glucocorticoids are also prohibited, but only when an athlete is in competition. A single class of compounds can contain a large number of prohibited substances and all of the compounds should be detected by the testing procedure. Since there are almost 70 stimulants on the prohibited list it can be a challenge to develop a single screening method that will optimally detect all the compounds. We describe a combined liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) testing method for detection of all the stimulants and narcotics on the World Anti-Doping Agency prohibited list. Urine for LC-MS/MS testing does not require sample pretreatment and is a direct dilute and shoot method. Urine samples for the GC-MS method require a liquid-liquid extraction followed by derivatization with trifluoroacetic anhydride.

Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

Directory of Open Access Journals (Sweden)

Mehdi Maham

2014-09-01

Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

Ultraviolet spectrophotometry of 2A 1822--371: A bulge on the accretion disk

International Nuclear Information System (INIS)

Mason, K.O.; Cordova, F.A.

1982-01-01

The X-ray source 2A 1822--371 has been observed with the IUE satellite over an 8 hour period. Long and short wavelength exposures of duration 45 or 60 minutes were alternated in order to resolve the 5.57 hr photometric modulation of the star. The data provide evidence that the shape of the 5.57 hr modulation evolves smoothly with energy between extremes defined by the optical and X-ray curves. The far-UV light curve is more deeply modulated than the X-ray light curve. The combined ultraviolet and the UBV band optical data can be fitted with a single blackbody of temperature 2.7 x 10 4 K, or an optically thick disk model with parameters T/sub asterisk/ = 1.2 x 10 5 K and R/sub out//R/sub in/approx.30. A single power-law model does not adequately represent the continuum. There is evidence of absorption due to the 2200 A interstellar feature whose depth requires a color excess, E(B--V)approx.0.1, with 3 sigma upper and lower bounds of 0.29 and 0.01. Emission lines of C IV 1550 A and N V 1240 A are detected in the UV spectrum. The work of Mason et al. and White et al. suggests that the optical and ultraviolet emission arises in an accretion disk, whereas the X-radiation is emitted from a scattering cloud that envelopes a central compact object. In the present paper, the 5.57 hr optical, X-ray and ultraviolet modulation of 2A 1822--371 is intrepreted as the result of partial occultation of the emitting region by a comparison star and a bulge on the outer accretion disk. X-ray heating of the bulge will probably also contribute to the modulation at optical and ultraviolet wavelengths

New type of discharge-produced plasma source for extreme ultraviolet based on liquid tin jet electrodes

NARCIS (Netherlands)

Koshelev, K.N.; Krivtsun, V.M.; Ivanov, V.; Yakushev, O.; Chekmarev, A.; Koloshnikov, V.; Snegirev, E.; Medvedev, Viacheslav

2012-01-01

A new approach for discharge-produced plasma (DPP) extreme ultraviolet (EUV) sources based on the usage of two liquid metallic alloy jets as discharge electrodes has been proposed and tested. Discharge was ignited using laser ablation of one of the cathode jets. A system with two jet electrodes was

Miniaturized protein separation using a liquid chromatography column on a flexible substrate

International Nuclear Information System (INIS)

Yang Yongmo; Chae, Junseok

2008-01-01

We report a prototype protein separator that successfully miniaturizes existing technology for potential use in biocompatible health monitoring implants. The prototype is a liquid chromatography (LC) column (LC mini-column) fabricated on an inexpensive, flexible, biocompatible polydimethylsiloxane (PDMS) enclosure. The LC mini-column separates a mixture of proteins using size exclusion chromatography (SEC) with polydivinylbenzene beads (5–20 µm in diameter with 10 nm pore size). The LC mini-column is smaller than any commercially available LC column by a factor of ∼11 000 and successfully separates denatured and native protein mixtures at ∼71 psi of the applied fluidic pressure. Separated proteins are analyzed using NuPAGE-gel electrophoresis, high-performance liquid chromatography (HPLC) and an automated electrophoresis system. Quantitative HPLC results demonstrate successful separation based on intensity change: within 12 min, the intensity between large and small protein peaks changed by a factor of ∼20. In further evaluation using the automated electrophoresis system, the plate height of the LC mini-column is between 36 µm and 100 µm. The prototype LC mini-column shows the potential for real-time health monitoring in applications that require inexpensive, flexible implant technology that can function effectively under non-laboratory conditions

Liquid chromatography and liquid chromatography-mass spectrometry analysis of donepezil degradation products

Directory of Open Access Journals (Sweden)

Mladenović Aleksandar R.

2015-01-01

Full Text Available This study describes the investigation of degradation products of donepezil (DP using stability indicating RP-HPLC method for determination of donepezil, which is a centrally acting reversible acetylcholinesterase inhibitor. In order to investigate the stability of drug and formed degradation products, a forced degradation study of drug sample and finished product under different forced degradation conditions has been conducted. Donepezil hydrochloride and donepezil tablets were subjected to stress degradation conditions recommended by International Conference on Harmonization (ICH. Donepezil hydrochloride solutions were subjected to acid and alkali hydrolysis, chemical oxidation and thermal degradation. Significant degradation was observed under alkali hydrolysis and oxidative degradation conditions. Additional degradation products were observed under the conditions of oxidative degradation. The degradation products observed during forced degradation studies were monitored using the high performance liquid chromatography (HPLC method developed. The parent method was modified in order to obtain LC-MS compatible method which was used to identify the degradation products from forced degradation samples using high resolution mass spectrometry. The mass spectrum provided the precise mass from which derived molecular formula of drug substance and degradation products formed and proved the specificity of the method unambiguously. [Projekat Ministarstva nauke Republike Srbije, br. 172013

Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

Directory of Open Access Journals (Sweden)

Pia Sala

2015-04-01

Full Text Available A novel liquid chromatography-mass spectrometry (LC-MS approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI coupled to hydrophilic interaction liquid chromatography (HILIC was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID fragment spectra in a linear ion trap. The process of chromatography development showed the best separation properties with a silica-based Kinetex column. This type of chromatography was able to separate all major lipid classes expected in mammalian samples, yielding increased sensitivity of oxidized phosphatidylcholines over reversed phase chromatography. Identification of molecular species was achieved by exact mass on intact molecular ions and CID tandem mass spectra containing characteristic fragments. Due to a lack of commercially available standards, method development was performed with copper induced oxidation products of palmitoyl-arachidonoyl-phosphatidylcholine, which resulted in a plethora of lipid species oxidized at the arachidonoyl moiety. Validation of the method was done with copper oxidized human low-density lipoprotein (LDL prepared by ultracentrifugation. In these LDL samples we could identify 46 oxidized molecular phosphatidylcholine species out of 99 possible candidates.

Description of Adsorption in Liquid Chromatography under Nonideal Conditions.

Science.gov (United States)

Ortner, Franziska; Ruppli, Chantal; Mazzotti, Marco

2018-05-15

A thermodynamically consistent description of binary adsorption in reversed-phase chromatography is presented, accounting for thermodynamic nonidealities in the liquid and adsorbed phases. The investigated system involves the adsorbent Zorbax 300SB-C18, as well as phenetole and 4- tert-butylphenol as solutes and methanol and water as inert components forming the eluent. The description is based on adsorption isotherms, which are a function of the liquid-phase activities, to account for nonidealities in the liquid phase. Liquid-phase activities are calculated with a UNIQUAC model established in this work, based on experimental phase equilibrium data. The binary interaction in the adsorbed phase is described by the adsorbed solution theory, assuming an ideal (ideal adsorbed solution theory) or real (real adsorbed solution theory) adsorbed phase. Implementation of the established adsorption model in a chromatographic code achieves a quantitative description of experimental elution profiles, with feed compositions exploiting the entire miscible region, and involving a broad range of different eluent compositions (methanol/water). The quantitative agreement of the model and experimental data serves as a confirmation of the underlying physical (thermodynamic) concepts and of their applicability to a broad range of operating conditions.

High-performance liquid chromatography separation of unsaturated organic compounds by a monolithic silica column embedded with silver nanoparticles.

Science.gov (United States)

Zhu, Yang; Morisato, Kei; Hasegawa, George; Moitra, Nirmalya; Kiyomura, Tsutomu; Kurata, Hiroki; Kanamori, Kazuyoshi; Nakanishi, Kazuki

2015-08-01

The optimization of a porous structure to ensure good separation performances is always a significant issue in high-performance liquid chromatography column design. Recently we reported the homogeneous embedment of Ag nanoparticles in periodic mesoporous silica monolith and the application of such Ag nanoparticles embedded silica monolith for the high-performance liquid chromatography separation of polyaromatic hydrocarbons. However, the separation performance remains to be improved and the retention mechanism as compared with the Ag ion high-performance liquid chromatography technique still needs to be clarified. In this research, Ag nanoparticles were introduced into a macro/mesoporous silica monolith with optimized pore parameters for high-performance liquid chromatography separations. Baseline separation of benzene, naphthalene, anthracene, and pyrene was achieved with the theoretical plate number for analyte naphthalene as 36,000 m(-1). Its separation function was further extended to cis/trans isomers of aromatic compounds where cis/trans stilbenes were chosen as a benchmark. Good separation of cis/trans-stilbene with separation factor as 7 and theoretical plate number as 76,000 m(-1) for cis-stilbene was obtained. The trans isomer, however, is retained more strongly, which contradicts the long- established retention rule of Ag ion chromatography. Such behavior of Ag nanoparticles embedded in a silica column can be attributed to the differences in the molecular geometric configuration of cis/trans stilbenes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a fully automated sequential injection solid-phase extraction procedure coupled to liquid chromatography to determine free 2-hydroxy-4-methoxybenzophenone and 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid in human urine.

Science.gov (United States)

León, Zacarías; Chisvert, Alberto; Balaguer, Angel; Salvador, Amparo

2010-04-07

2-Hydroxy-4-methoxybenzophenone and 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid, commonly known as benzophenone-3 (BZ3) and benzophenone-4 (BZ4), respectively, are substances widely used as UV filters in cosmetic products in order to absorb UV radiation and protect human skin from direct exposure to the deleterious wavelengths of sunlight. As with other UV filters, there is evidence of their percutaneous absorption. This work describes an analytical method developed to determine trace levels of free BZ3 and BZ4 in human urine. The methodology is based on a solid-phase extraction (SPE) procedure for clean-up and pre-concentration, followed by the monitoring of the UV filters by liquid chromatography-ultraviolet spectrophotometry detection (LC-UV). In order to improve not only the sensitivity and selectivity, but also the precision of the method, the principle of sequential injection analysis was used to automate the SPE process and to transfer the eluates from the SPE to the LC system. The application of a six-channel valve as an interface for the switching arrangements successfully allowed the on-line connection of SPE sample processing with LC analysis. The SPE process for BZ3 and BZ4 was performed using octadecyl (C18) and diethylaminopropyl (DEA) modified silica microcolumns, respectively, in which the analytes were retained and eluted selectively. Due to the matrix effects, the determination was based on standard addition quantification and was fully validated. The relative standard deviations of the results were 13% and 6% for BZ3 and BZ4, respectively, whereas the limits of detection were 60 and 30 ng mL(-1), respectively. The method was satisfactorily applied to determine BZ3 and BZ4 in urine from volunteers that had applied a sunscreen cosmetic containing both UV filters. Copyright 2010 Elsevier B.V. All rights reserved.

Development of a fully automated sequential injection solid-phase extraction procedure coupled to liquid chromatography to determine free 2-hydroxy-4-methoxybenzophenone and 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid in human urine

International Nuclear Information System (INIS)

Leon, Zacarias; Chisvert, Alberto; Balaguer, Angel; Salvador, Amparo

2010-01-01

2-Hydroxy-4-methoxybenzophenone and 2-hydroxy-4-methoxybenzophenone-5-sulphonic acid, commonly known as benzophenone-3 (BZ3) and benzophenone-4 (BZ4), respectively, are substances widely used as UV filters in cosmetic products in order to absorb UV radiation and protect human skin from direct exposure to the deleterious wavelengths of sunlight. As with other UV filters, there is evidence of their percutaneous absorption. This work describes an analytical method developed to determine trace levels of free BZ3 and BZ4 in human urine. The methodology is based on a solid-phase extraction (SPE) procedure for clean-up and pre-concentration, followed by the monitoring of the UV filters by liquid chromatography-ultraviolet spectrophotometry detection (LC-UV). In order to improve not only the sensitivity and selectivity, but also the precision of the method, the principle of sequential injection analysis was used to automate the SPE process and to transfer the eluates from the SPE to the LC system. The application of a six-channel valve as an interface for the switching arrangements successfully allowed the on-line connection of SPE sample processing with LC analysis. The SPE process for BZ3 and BZ4 was performed using octadecyl (C18) and diethylaminopropyl (DEA) modified silica microcolumns, respectively, in which the analytes were retained and eluted selectively. Due to the matrix effects, the determination was based on standard addition quantification and was fully validated. The relative standard deviations of the results were 13% and 6% for BZ3 and BZ4, respectively, whereas the limits of detection were 60 and 30 ng mL -1 , respectively. The method was satisfactorily applied to determine BZ3 and BZ4 in urine from volunteers that had applied a sunscreen cosmetic containing both UV filters.

Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

Science.gov (United States)

Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

2016-10-01

The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of Grayanotoxins from Rhododendron brachycarpum in Dietary Supplements and Homemade Wine by Liquid Chromatography-Quadrupole Time-of-Flight-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry.

Science.gov (United States)

Hwang, Taeik; Noh, Eunyoung; Jeong, Ji Hye; Park, Sung-Kwan; Shin, Dongwoo; Kang, Hoil

2018-02-28

A sensitive and specific high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry (LC-QTOF-MS) method combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of grayanotoxins I and III in dietary supplements and homemade wine. Grayanotoxins I and III were successfully extracted using solid-phase extraction cartridges, characterized by LC-QTOF-MS, and quantitated by LC-MS/MS. The LC-MS/MS calibration curves were linear over concentrations of 10-100 ng/mL (grayanotoxin I) and 20-400 ng/mL (grayanotoxin III). Grayanotoxins I and III were found in 51 foodstuffs, with quantitative determinations revealing total toxin concentrations of 18.4-101 000 ng/mL (grayanotoxin I) and 15.3-56 000 ng/mL (grayanotoxin III). The potential of the validated method was demonstrated by successful quantitative analysis of grayanotoxins I and III in dietary supplements and homemade wine; the method appears suitable for the routine detection of grayanotoxins I and III from Rhododendron brachycarpum.

High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

Science.gov (United States)

Haddad, Paul; And Others

1983-01-01

Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

Application and recovery of ionic liquids in the preparative separation of four flavonoids from Rhodiola rosea by on-line three-dimensional liquid chromatography.

Science.gov (United States)

Ma, Shufeng; Hu, Liming; Ma, Chaoyang; Lv, Wenping; Wang, Hongxin

2014-09-01

A novel on-line three-dimensional liquid chromatography method was developed to separate four main flavonoids from Rhodiola rosea. Ethyl acetate/0.5 mol/L ionic liquid 1-butyl-3-methylimidazolium chloride aqueous solution was selected as the solvent system. In the first-dimension separation, the target flavonoids were entrapped and subsequently desorbed into the second-dimension high-speed countercurrent chromatographic column for separation. In the third-dimension chromatography, the residual ionic liquid in the four separated flavonoids was removed and the used ionic liquid was recovered. As a result, 35.1 mg of compound 1, 20.4 mg of compound 2, 8.5 mg of compound 3, and 10.6 mg of compound 4 were obtained from 1.53 g R. rosea extract. They were identified as rhodiosin, rhodionin, herbacetin, and kaempferol, respectively. The recovery of ionic liquid reached 99.1% of the initial amount. The results showed that this method is a powerful technology for the separation of R. rosea flavonoids and that the ionic-liquid-based solvent system has advantages over traditional solvent systems in renewable and environmentally friendly properties. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

International Nuclear Information System (INIS)

Lamouroux, C.

2011-01-01

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

Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

Science.gov (United States)

Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

2017-11-24

Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

Ionic-liquid-based ultrasound-assisted extraction of isoflavones from Belamcanda chinensis and subsequent screening and isolation of potential α-glucosidase inhibitors by ultrafiltration and semipreparative high-performance liquid chromatography.

Science.gov (United States)

Li, Senlin; Li, Sainan; Huang, Yu; Liu, Chunming; Chen, Lina; Zhang, Yuchi

2017-06-01

The separation of a compound of interest from its structurally similar homologues to produce high-purity natural products is a challenging problem. This work proposes a novel method for the separation of iristectorigenin A from its structurally similar homologues by ionic-liquid-based ultrasound-assisted extraction and the subsequent screening and isolation of potential α-glucosidase inhibitors via ultrafiltration and semipreparative high-performance liquid chromatography. Ionic-liquid-based ultrasound-assisted extraction was successfully applied to the extraction of tectorigenin, iristectorigenin A, irigenin, and irisflorentin from Belamcanda chinensis. The optimum conditions for the efficient extraction of isoflavones were determined as 1.0 M 1-ethyl-3-methylimidazolium tetrafluoroborate with extraction time of 30 min and a solvent to solid ratio of 30 mL/g. Ultrafiltration with liquid chromatography and mass spectrometry was applied to screen and identify α-glucosidase inhibitors from B. chinensis, followed by the application of semipreparative high-performance liquid chromatography to separate and isolate the active constituents. Four major compounds including tectorigenin, iristectorigenin A, irigenin, and irisflorentin were screened and identified as α-glucosidase inhibitors, and then the four active compounds abovementioned were subsequently isolated by semipreparative high-performance liquid chromatography (99.89, 88.97, 99.79, and 99.97% purity, respectively). The results demonstrate that ionic liquid extraction can be successfully applied to the extraction of isoflavones from B. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of lanthanum from nuclear fuel solutions by high performance liquid chromatography

International Nuclear Information System (INIS)

Lazar, G. C.; Petre, M.; Androne, G.; Benga, A.

2016-01-01

This paper presents the separation of uranium, praseodymium and lanthanum from nuclear fuel solutions by high performance liquid chromatography (HPLC). The aim of this study is to establish a minimum concentration of lanthanum which can be analyzed by high performance liquid chromatography, and also to study the effect of uranium concentration on the separation of praseodymium and lanthanum. Optimum gradient mode was established for mixture standard stoc solutions with uranium in a concentration of 1 mg/ml, praseodymium and lanthanum in a concentration range of 1-5 μg/ml from each element. These conditions were applied for the separation of lanthanum from a nuclear fuel solution in which praseodymium and lanthanum were added in a concentration of 3 μg/ml from each element. The elution behavior of lanthanum as a function of the pH and the concentration of the mobile phase, using a mixture of 1-octanesulfonic acid sodium salt with a-hidroxyisobutiric acid is presented. (authors)

Fingerprint analysis of Resina Draconis by ultra-performance liquid chromatography

OpenAIRE

Xue, Yudi; Zhu, Lin; Yi, Tao

2017-01-01

Background Resina Draconis, a bright red resin derived from Dracaena cochinchinensis, is a traditional medicine used in China. To improve its quality control approach, an ultra-performance liquid chromatography (UPLC) fingerprint method was developed for rapidly evaluating the quality of Resina Draconis. Methods The precision, repeatability and stability of the proposed UPLC method were validated in the study. Twelve batches of Resina Draconis samples from various sources were analyzed by the...

高效液相色谱-紫外检测法测定水产品中组胺含量%Determination of histamine content in aquatic products by high performance liquid chromatography with ultraviolet detector

Institute of Scientific and Technical Information of China (English)

徐丽; 刘琳; 王宗奇; 孟慧琴; 张雪琰

2014-01-01

Objective To improve the method of high performance liquid chromatography (HPLC) for determination of histamine in aquatic product (mackerel fish), and to develop a method with simple extraction, stable derivatives, and easy to operate.Method The perchloric acid solution 0.4 mol/L was used to extract histamine of aquatic products, dansyl chloride solution 10 mg/mL as derivative agent, methanol and water as the HPLC flow phase to gradient elution. The histamine content was detected by high performance liquid chromatography with ultraviolet detector.Results The method had the advantages of complete extraction, simple operation, ideal peak, less interference of histamine peak. The recovery rate was more than 90%, and the detection limit was 50 mg/kg.Conclusion It can meet the requirements of determination of histamine in aquatic products, and is an ideal method for detection of histamine.%目的：对高效液相色谱法测定水产品(鲭鱼)中组胺含量的试验方法进行改进，建立一种提取方法简单、衍生物稳定、操作方便的检测方法。方法用0.4 mol/L高氯酸溶液提取水产品中的组胺，采用10 mg/mL丹磺酰氯溶液作为衍生剂进行衍生，用甲醇、水的流动相梯度洗脱，高效液相色谱-紫外检测法测定水产品中的组胺含量。结果该方法提取完全、操作简单、峰型理想、组胺出峰干扰少，回收率大于90%，方法检出限为50 mg/kg。结论该方法能够满足水产品中组胺含量的测定要求，是一种理想的组胺检测方法。

Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

International Nuclear Information System (INIS)

Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

1995-01-01

The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

Monoliths in capillary electrochromatography and capillary liquid chromatography in conjunction with mass spectrometry

Czech Academy of Sciences Publication Activity Database

Moravcová, Dana; Rantamäki, A. H.; Duša, Filip; Wiedmer, S. K.

2016-01-01

Roč. 37, 7-8 (2016), s. 880-912 ISSN 0173-0835 Institutional support: RVO:68081715 Keywords : capillary electrochromatography * capillary liquid chromatography * mass spec- trometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.744, year: 2016

Analysis of polymeric phenolics in red wines using different techniques combined with gel permeation chromatography fractionation.

Science.gov (United States)

Guadalupe, Zenaida; Soldevilla, Alberto; Sáenz-Navajas, María-Pilar; Ayestarán, Belén

2006-04-21

A multiple-step analytical method was developed to improve the analysis of polymeric phenolics in red wines. With a common initial step based on the fractionation of wine phenolics by gel permeation chromatography (GPC), different analytical techniques were used: high-performance liquid chromatography-diode array detection (HPLC-DAD), HPLC-mass spectrometry (MS), capillary zone electrophoresis (CZE) and spectrophotometry. This method proved to be valid for analyzing different families of phenolic compounds, such as monomeric phenolics and their derivatives, polymeric pigments and proanthocyanidins. The analytical characteristics of fractionation by GPC were studied and the method was fully validated, yielding satisfactory statistical results. GPC fractionation substantially improved the analysis of polymeric pigments by CZE, in terms of response, repeatability and reproducibility. It also represented an improvement in the traditional vanillin assay used for proanthocyanidin (PA) quantification. Astringent proanthocyanidins were also analyzed using a simple combined method that allowed these compounds, for which only general indexes were available, to be quantified.

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

Science.gov (United States)

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

2017-12-01

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

Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

Science.gov (United States)

Lee, Iris; Boyce, Mary C.

2011-01-01

A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

A theoretical analysis of the ultraviolet spectrum (180-260 nm) of pure liquid benzene

International Nuclear Information System (INIS)

Fernandez, M.; Tortajada, J.; Sese, L.M.

1988-01-01

This paper reports an attempt to understand theoretically the red shifts seen in the benzene ultraviolet spectrum upon changing from gas to the liquid phase. The theoretical analysis is performed through a framework which brings together Quantum Chemistry and Classical Statistical Mechanics of molecular liquids. As it is discussed herein, the influence of the liquid phase on the individual molecular properties is taken into account by means of a perturbation term included in the effective molecular Hamiltonian. Such a perturbation depends explicitly on both the chemical nature and the static structure of the liquid surrounding the molecule under study. In order to simulate the vibronic couplings, which make the benzene ''forbidden'' bands 1 L a and 1 L b have nonzero intensity, random displacements of the nuclei of benzene have been employed in this introductory work. The calculations involve the CNDO/S procedure and the atom-atom radial distribution functions of the liquid sample. The results account for the large red shift (≅ 20 nm) undergone by the band 1 L a . (orig.)

Characterization of Extracellular Vesicles by Size-Exclusion High-Performance Liquid Chromatography (HPLC).

Science.gov (United States)

Huang, Tao; He, Jiang

2017-01-01

Extracellular vesicles (EVs) have recently attracted substantial attention due to the potential diagnostic and therapeutic relevance. Although a variety of techniques have been used to isolate and analyze EVs, it is still far away from satisfaction. Size-exclusion chromatography (SEC), which separates subjects by size, has been widely applied in protein purification and analysis. The purpose of this chapter is to show the applications of size-exclusion high-performance liquid chromatography (HPLC) as methods for EV characterization of impurities or contaminants of small size, and thus for quality assay for the purity of the samples of EVs.

Urinary neopterin quantification by reverse-phase high-performance liquid chromatography with ultraviolet detection

NARCIS (Netherlands)

Castro, de M.R.; Marco, Di G.S.; Arita, D.Y.; Teixeira, L.C.; Pereira, A.B.; Casarini, D.E.

2004-01-01

Neopterin plays an important role in the malignant disease diagnostics. However, the methods employed in neopterin determination are generally difficult and/or time consuming. The aim of this work was to standardize a practical method to quantify neopterin using high-performance liquid

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

NARCIS (Netherlands)

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

1983-01-01

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

Determination of Peroxide-Based Explosives Using Liquid Chromatography with On-Line Infrared Detection

NARCIS (Netherlands)

Schulte-Ladbeck, Rasmus; Edelmann, Andrea; Quintas, Guillermo; Lendl, Bernhard; Karst, U.

2006-01-01

A nondestructive analytical method for peroxide-based explosives determination in solid samples is described. Reversed-phase high-performance liquid chromatography in combination with on-line Fourier transform infrared (FT-IR) detection is used for the analysis of triacetonetriperoxide (TATP) and

Quantification of liquid products from the electroreduction of CO2 and CO using static headspace-gas chromatography and nuclear magnetic resonance spectroscopy

DEFF Research Database (Denmark)

Bertheussen, Erlend; Abghoui, Younes; Jovanov, Zarko P.

2017-01-01

Static headspace-gas chromatography (HS-GC) useful for ex-situ liquid product analysis. Could complement high-performance liquid chromatography and NMR spectroscopy. Particularly high sensitivity towards compounds with high vapor pressure. Detection limits below 0.5μM were shown for acetaldehyde...

Nanoparticle Analysis by Online Comprehensive Two-Dimensional Liquid Chromatography combining Hydrodynamic Chromatography and Size-Exclusion Chromatography with Intermediate Sample Transformation

Science.gov (United States)

2017-01-01

Polymeric nanoparticles have become indispensable in modern society with a wide array of applications ranging from waterborne coatings to drug-carrier-delivery systems. While a large range of techniques exist to determine a multitude of properties of these particles, relating physicochemical properties of the particle to the chemical structure of the intrinsic polymers is still challenging. A novel, highly orthogonal separation system based on comprehensive two-dimensional liquid chromatography (LC × LC) has been developed. The system combines hydrodynamic chromatography (HDC) in the first-dimension to separate the particles based on their size, with ultrahigh-performance size-exclusion chromatography (SEC) in the second dimension to separate the constituting polymer molecules according to their hydrodynamic radius for each of 80 to 100 separated fractions. A chip-based mixer is incorporated to transform the sample by dissolving the separated nanoparticles from the first-dimension online in tetrahydrofuran. The polymer bands are then focused using stationary-phase-assisted modulation to enhance sensitivity, and the water from the first-dimension eluent is largely eliminated to allow interaction-free SEC. Using the developed system, the combined two-dimensional distribution of the particle-size and the molecular-size of a mixture of various polystyrene (PS) and polyacrylate (PACR) nanoparticles has been obtained within 60 min. PMID:28745485

Chromatography Of Metal Ions On Wood Cellulose Impregnated ...

African Journals Online (AJOL)

Adsorption chromatography of some heavy metal ions on wood cellulose of saw dust (wood waste dust) modified with hydrochloric acid, urea and thiourea was studied. Atomic absorption spectrophotometry (AAS) was used to determine the initial concentration of solutions of Zn2+, Cu2+, Ni2+, Pb2+, and Fe3+ metal ions.

Greening Reversed-Phase Liquid Chromatography Methods Using Alternative Solvents for Pharmaceutical Analysis

Directory of Open Access Journals (Sweden)

Moussa Yabré

2018-05-01

Full Text Available The greening of analytical methods has gained increasing interest in the field of pharmaceutical analysis to reduce environmental impacts and improve the health safety of analysts. Reversed-phase high-performance liquid chromatography (RP-HPLC is the most widely used analytical technique involved in pharmaceutical drug development and manufacturing, such as the quality control of bulk drugs and pharmaceutical formulations, as well as the analysis of drugs in biological samples. However, RP-HPLC methods commonly use large amounts of organic solvents and generate high quantities of waste to be disposed, leading to some issues in terms of ecological impact and operator safety. In this context, greening HPLC methods is becoming highly desirable. One strategy to reduce the impact of hazardous solvents is to replace classically used organic solvents (i.e., acetonitrile and methanol with greener ones. So far, ethanol has been the most often used alternative organic solvent. Others strategies have followed, such as the use of totally aqueous mobile phases, micellar liquid chromatography, and ionic liquids. These approaches have been well developed, as they do not require equipment investments and are rather economical. This review describes and critically discusses the recent advances in greening RP-HPLC methods dedicated to pharmaceutical analysis based on the use of alternative solvents.

The high pressure liquid chromatography and its application to the separation of polynuclear aromatic hydrocarbons in atmospheric dust and burning residues

International Nuclear Information System (INIS)

Lopez, M.-C.

1975-09-01

A new technique of analysis is described: the high speed liquid chromatography or more exactly the high performance liquid chromatography because of the progress achieved on the new packings of the columns. The main types of chromatography, according to the phenomena involved are described: adsorption, partition, ion-exchange and exclusion chromatography. A brief outline is given of the theory for determination of stationary and mobile phases in order to obtain the optimum conditions of separation. Some exemples of possible applications are given, particularly the use of this technique for the separation of polycyclic aromatic hydrocarbons in atmospheric pollution and burning residues [fr

Determination of ibuprofen enantiomers in breast milk using vortex-assisted matrix solid-phase dispersion and direct chiral liquid chromatography.

Science.gov (United States)

León-González, M E; Rosales-Conrado, N

2017-09-08

A mixture of β-cyclodextrin (β-CD) and primary and secondary amine (PSA) sorbents was employed for the extraction and quantification of ibuprofen enantiomers from human breast milk, combining a vortex-assisted matrix solid-phase dispersion method (MSPD) and direct chiral liquid chromatography (CLC) with ultraviolet detection (UV). The MSPD sample preparation procedure was optimized focusing on both the type and amount of dispersion/sorption sorbents and the nature of the elution solvent, in order to obtain acceptable recoveries and avoiding enantiomer conversion. These MSPD parameters were optimized with the aid of an experimental design approach. Hence, a factorial design was used for identification of the main variables affecting the extraction process of ibuprofen enantiomers. Under optimum selected conditions, MSPD combined with direct CLC-UV was successfully applied for ibuprofen enantiomeric determination in breast milk at enantiomer levels between 0.15 and 6.0μgg -1 . The proposed analytical method also provided good repeatability, with relative standard deviations of 6.4% and 8.3% for the intra-day and inter-day precision, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of parabens in serum by liquid chromatography-tandem mass spectrometry: Correlation with lipstick use.

Science.gov (United States)

Tahan, Gabriella Padovani; Santos, Nayara de Kássia Souza; Albuquerque, Ana Carolina; Martins, Isarita

2016-08-01

Parabens are the most widely used preservative and are considered to be relatively safe compounds. However, studies have demonstrated that they may have estrogenic activity, and there is ongoing debate regarding the safety and potential cancer risk of using products containing these compounds. In the present work, liquid chromatography-tandem mass spectrometry was applied to determine methylparaben and propylparaben concentrations in serum, and the results were correlated with lipstick application. Samples were analyzed using liquid-liquid extraction, followed by liquid chromatography-tandem mass spectrometry. The validation results demonstrated the linearity of the method over a range of 1-20 ng/mL, in addition to the method's precision and accuracy. A statistically significant difference was demonstrated between serum parabens in women who used lipstick containing these substances compared with those not using this cosmetic (p = 0.0005 and 0.0016, respectively), and a strong association was observed between serum parabens and lipstick use (Spearman correlation = 0.7202). Copyright © 2016 Elsevier Inc. All rights reserved.

Simultaneous analysis of aspartame and its hydrolysis products of Coca-Cola Zero by on-line postcolumn derivation fluorescence detection and ultraviolet detection coupled two-dimensional high-performance liquid chromatography.

Science.gov (United States)

Cheng, Cheanyeh; Wu, Shing-Chen

2011-05-20

An innovative two-dimensional high-performance liquid chromatography system was developed for the simultaneous analysis of aspartame and its hydrolysis products of Coca-Cola Zero. A C8 reversed-phase chromatographic column with ultraviolet detection was used as the first dimension for the determination of aspartame, and a ligand-exchange chromatographic column with on-line postcolumn derivation fluorescence detection was employed as the second dimension for the analysis of amino acid enantiomers. The fluorimetric derivative reagent of amino acid enantiomers was o-phthaldialdehyde. The hydrolysis of aspartame in Coca-Cola Zero was induced by electric-heating or microwave heating. Aspartame was quantified by the matrix matched external standard calibration curve with a linear concentration range of 0-50 μg mL(-1) (r(2)=0.9984). The limit of detection (LOD) and the limit of quantification (LOQ) were 1.3 μg mL(-1) and 4.3 μg mL(-1), respectively. The amino acid enantiomers was analyzed by the matrix matched internal standard calibration method (D-leucine as the internal standard) with a linear concentration range of 0-10 μg mL(-1) (r(2)=0.9988-0.9997). The LODs and LOQs for L- and D-aspartic acid and L- and D-phenylalanine were 0.16-0.17 μg mL(-1) and 0.52-0.55 μg mL(-1), respectively, that was 12-13 times more sensitive than ultraviolet detection. The overall analysis accuracy for aspartame and amino acid enantiomers was 90.2-99.2% and 90.4-96.2%, respectively. The overall analysis precision for aspartame and amino acid enantiomers was 0.1-1.7% and 0.5-6.7%, respectively. Generally, the extent of aspartame hydrolysis increases with the increase of electro-thermal temperature, microwave power, and the duration of hydrolysis time. D-aspartic acid and D-phenylalanine can be observed with the electro-thermal racemization at the hydrolysis temperature 120°C for 1 day and only D-aspartic acid can be observed at the hydrolysis temperature 90°C for 2 and 3 days. For

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

Science.gov (United States)

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.

Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

Science.gov (United States)

Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

2015-09-01

In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Science.gov (United States)

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

Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics

OpenAIRE

Pacakova, V.; Leclercq, P.A.

1991-01-01

The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the prod...

Qualitative and quantitative determination of ubiquinones by the method of high-efficiency liquid chromatography

International Nuclear Information System (INIS)

Yanotovskii, M.T.; Mogilevskaya, M.P.; Obol'nikova, E.A.; Kogan, L.M.; Samokhvalov, G.I.

1986-01-01

A method has been developed for the qualitative and quantitative determination of ubiquinones CoQ 6 -CoQ 10 , using high-efficiency reversed-phase liquid chromatography. Tocopherol acetate was used as the internal standard

Analysis of penicillin G in milk by liquid chromatography.

Science.gov (United States)

Boison, J O; Keng, L J; MacNeil, J D

1994-01-01

A liquid chromatographic (LC) method that was previously developed for penicillin G residues in animal tissues has been adapted to milk and milk products. After protein precipitation with sodium tungstate, samples are applied to a C18 solid-phase extraction cartridge, from which penicillin is eluted, derivatized with 1,2,4-triazole-mercuric chloride solution, and analyzed by isocratic liquid chromatography (LC) on a C18 column with UV detection at 325 nm. Quantitation is done with reference to penicillin V as an internal standard. Penicillin G recoveries were determined to be > 70% on standards fortified at 3-60 ppb. Accuracy approached 100% using the penicillin V internal standard. The detection limit for penicillin G residues was 3 ppb in fluid milk. Samples may be confirmed by thermospray/LC at concentrations approaching the detection limit of the UV method.

Group type analysis of asphalt by column liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Zhang, C.; Yang, J.; Xue, Y.; Li, Y. [Chinese Academy of Science, Taiyuan (China)

2008-07-01

An improved analysis method for characterization of asphalt was established. The method is based on column chromatography technique. The asphalts were separated into four groups: saturates, aromatics, resins, and asphaltenes, quantitatively. About 0.1 g of sample was required in each analysis. About 20 mL of n-heptanes was used to separate out saturates first. Then about 35 mL of n-heptanes/dichloromethane (.5, v/v) mixture was used to separate out aromatics. About 30 mL of dichloromethane/tetrahydrofuran (1/3, v/v) mixture was used to separate out resin. The quality of the separation was confirmed by infrared spectra (IR) and {sup 1}H NMR analysis. The model compounds, tetracosan for saturates, dibenz(o)anthracen for aromatics, and acetanilide for resins were used for verification. The IR and {sup 1}H NMR analysis of the prepared fractions from the column liquid chromatography were in good agreement that of pure reagents.

Characterization of pitches by liquid chromatography using cellulose 3,5-dinitrobenzoate as the packing material

Energy Technology Data Exchange (ETDEWEB)

Arai, K.; Judo, R.; Ota, E. [Gunma University, Gunma (Japan). Dept. of Chemistry

1997-08-01

Characterization of coal tar, petroleum and PVC pitches by a liquid chromatography using cellulose 3,5-dinitrobenzoate (DNB-cellulose) as the packing material was investigated. Separation mechanism based on charge-transfer interaction between the dinitrobenzoyl group and polyaromatic compounds was expected to be useful for separation of the constituents of the pitches. First, 26 model polyaromatic compounds were tested to examine the characteristic feature of the packing material by liquid chromatography. The compounds were found to be classified roughly into four groups with different retention volume, principally according to the number of condensed rings. The nonplanar structure and aliphatic side chain of the polyaromatic compounds also affected the separation behavior. Both benzene soluble-hexane soluble and benzene soluble-hexane insoluble fractions of the three pitches were separated on DNB-cellulose. It was found that coal tar pitch contains relatively large amounts of some highly condensed polyaromatic compounds with condensed rings of 4 to 5; petroleum pitch has small amounts of such specific highly condensed polyaromatic compounds, while PVC pitch has large amounts of less condensed polyaromatic compounds and there is no significant amount of highly condensed compound in it. Thus DNB-cellulose was useful as the convenient packing material for liquid chromatography to characterize pitches.

Polydimethylsiloxane/covalent triazine frameworks coated stir bar sorptive extraction coupled with high performance liquid chromatography-ultraviolet detection for the determination of phenols in environmental water samples.

Science.gov (United States)

Zhong, Cheng; He, Man; Liao, Huaping; Chen, Beibei; Wang, Cheng; Hu, Bin

2016-04-08

In this work, covalent triazine frameworks (CTFs) were introduced in stir bar sorptive extraction (SBSE) and a novel polydimethylsiloxane(PDMS)/CTFs stir bar coating was prepared by sol-gel technique for the sorptive extraction of eight phenols (including phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-chloro-m-cresol and 2,4-dichlorophenol, 2,4,6-trichlorophenol) from environmental water samples followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. The prepared PDMS/CTFs coated stir bar showed good preparation reproducibility with the relative standard deviations (RSDs) ranging from 3.5 to 5.7% (n=7) in one batch, and from 3.7 to 9.3% (n=7) among different batches. Several parameters affecting SBSE of eight target phenols including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.08-0.30 μg/L. The linear range was 0.25-500 μg/L for 2-nitrophenol, 0.5-500 μg/L for phenol, 2-chlorophenol, 4-nitrophenol as well as 2,4-dimethylphenol, and 1-500 μg/L for p-chloro-m-cresol, 2,4-dichlorophenol as well as 2,4,6-trichlorophenol, respectively. The intra-day relative standard deviations (RSDs) were in the range of 4.3-9.4% (n=7, c=2 μg/L) and the enrichment factors ranged from 64.9 to 145.6 fold (theoretical enrichment factor was 200-fold). Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/CTFs stir bar showed better extraction efficiency for target phenol compounds. The proposed method was successfully applied to the analysis of phenols in environmental water samples and good relative recoveries were obtained with the spiking level at 2, 10, 50 μg/L, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

2008-07-11

Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method developed was successfully applied for primary screening of RTILs (>20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media.

Determination of ten carbamate pesticides in aquatic and sediment samples by liquid chromatography-ionspray and thermospray mass spectrometry.

NARCIS (Netherlands)

Honing, M.; Riu, J.; Barceló, D.; van Baar, B.L.M.; Brinkman, U.A.T.

1996-01-01

Ten carbamate pesticides which exhibit large differences in polarity were determined simultaneously in various environmental samples, using both column liquid chromatography (LC)-thermospray (TSP) mass spectrometry (MS) and LC-ionspray (ISP) MS. For sample clean-up, column chromatography with three

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

Science.gov (United States)

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

2016-01-01

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

Ultraviolet Spectroscopy of Asteroid(4) Vesta

Science.gov (United States)

Li, Jian-Yang; Bodewits, Dennis; Feaga, Lori M.; Landsman, Wayne; A'Hearn, Michael F.; Mutchler, Max J.; Russell, Christopher T.; McFadden, Lucy A.; Raymond, Carol A.

2011-01-01

We report a comprehensive review of the UV-visible spectrum and rotational lightcurve of Vesta combining new observations by Hubble Space Telescope and Swift with archival International Ultraviolet Explorer observations. The geometric albedos of Vesta from 220 nm to 953 nm arc derived by carefully comparing these observations from various instruments at different times and observing geometries. Vesta has a rotationally averaged geometric albedo of 0.09 at 250 nm, 0.14 at 300 nm, 0.26 at 373 nm, 0.38 at 673 nm, and 0.30 at 950 nm. The linear spectral slope in the ultraviolet displays a sharp minimum ncar sub-Earth longitude of 20deg, and maximum in the eastern hemisphere. This is completely consistent with the distribution of the spectral slope in the visible wavelength. The uncertainty of the measurement in the ultraviolet is approx.20%, and in the visible wavelengths better than 10%. The amplitude of Vesta's rotational lightcurves is approx.10% throughout the range of wavelengths we observed, but is smaller at 950 nm (approx.6%) ncar the 1-micron mafic band center. Contrary to earlier reports, we found no evidence for any difference between the phasing of the ultraviolet and visible/ncar-infrared lightcurves with respect to sub-Earth longitude. Vesta's average spectrum between 220 and 950 nm can well be described by measured reflectance spectra of fine particle howardite-like materials of basaltic achondrite meteorites. Combining this with the in-phase behavior of the ultraviolet, visible. and ncar-infrared lightcurves, and the spectral slopes with respect to the rotational phase, we conclude that there is no global ultraviolet/visible reversal on Vesta. Consequently, this implies lack of global space weathering on Vesta. Keyword,: Asteroid Vesta; Spectrophotometry; Spectroscopy; Ultraviolet observations; Hubble Space Telescope observations

Isotope Fractionation in Methane Reactions Studied by Gas Chromatography and Liquid Scintillation

DEFF Research Database (Denmark)

Andersen, Bertel Lohmann; Bidoglio, G.; Leip, A.

1997-01-01

Determination of C-14-marked methane by gas chromatography and liquid scintillation counting is shown to be useful in studies of isotope effects. Data on the specific activity is used to separate the contributions of (CH4)-C-14, and (CH4)-C-12 to the gas-chromatographic peak area. As an application...

Assay of free urinary cortisol with inverted phase liquid chromatography and radiocompetition

International Nuclear Information System (INIS)

Franck, C.; Patricot, M.C.; Mathian, B.; Revol, A.

1984-01-01

The authors present an assay method for free urinary cortisol using inverted phase liquid chromatography for purification and radiocompetition for the assay. The usual values for adult men and women were established. The results of 150 routine assays were compared with those of 17 OHCS revealing the value of this assay [fr

A novel green chemistry method for nonaqueous extraction and high-performance liquid chromatography detection of first-, second-, and third-generation tetracyclines, 4-epitetracycline, and tylosin in animal feeds.

Science.gov (United States)

Granados-Chinchilla, Fabio; Sánchez, Jorge; García, Fernando; Rodríguez, César

2012-07-25

Although tetracyclines and macrolides are common additives for animal nutrition, methods for their simultaneous determination in animal feeds are nonexistent. By coupling an organic extraction and solid-phase extraction cleanup to a high-performance liquid chromatography separation and a nonaqueous postcolumn derivatization, we succeeded in detecting from 0.2 to 24.0 μg kg(-1) of tetracycline, oxytetracycline, chlortetracycline, doxycycline, tigecycline, and 4-epitetracycline in this complex and heterogeneous matrix. Minocycline and tylosin could also be detected with our procedure, but using UV spectrophotometry (1.5 ≤ LOD ≤ 1.9 mg kg(-1)). Linear responses with correlation coefficients between 0.996 and 0.999 were obtained for all analytes in the 0.5-10 mg kg(-1) concentration range. Average recoveries between 59 and 97% and between 98 and 102% were obtained for the tetracyclines and tylosin, respectively. Replicate standard deviations were typically below 5%. When this method was applied to 20 feeds marketed in Costa Rica, we detected labeling inconsistencies, banned mixtures of tetracyclines, and tetracycline concentrations that contravene international regulation.

Enantiomeric high-performance liquid chromatography resolution and absolute configuration of 6β-benzoyloxy-3α-tropanol.

Science.gov (United States)

Muñoz, Marcelo A; González, Natalia; Joseph-Nathan, Pedro

2016-07-01

The absolute configuration of the naturally occurring isomers of 6β-benzoyloxy-3α-tropanol (1) has been established by the combined use of chiral high-performance liquid chromatography with electronic circular dichroism detection and optical rotation detection. For this purpose (±)-1, prepared in two steps from racemic 6-hydroxytropinone (4), was subjected to chiral high-performance liquid chromatography with electronic circular dichroism and optical rotation detection allowing the online measurement of both chiroptical properties for each enantiomer, which in turn were compared with the corresponding values obtained from density functional theory calculations. In an independent approach, preparative high-performance liquid chromatography separation using an automatic fraction collector, yielded an enantiopure sample of OR (+)-1 whose vibrational circular dichroism spectrum allowed its absolute configuration assignment when the bands in the 1100-950 cm(-1) region were compared with those of the enantiomers of esters derived from 3α,6β-tropanediol. In addition, an enantiomerically enriched sample of 4, instead of OR (±)-4, was used for the same transformation sequence, whose high-performance liquid chromatography follow-up allowed their spectroscopic correlation. All evidences lead to the OR (+)-(1S,3R,5S,6R) and OR (-)-(1R,3S,5R,6S) absolute configurations, from where it follows that samples of 1 isolated from Knightia strobilina and Erythroxylum zambesiacum have the OR (+)-(1S,3R,5S,6R) absolute configuration, while the sample obtained from E. rotundifolium has the OR (-)-(1R,3S,5R,6S) absolute configuration. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Expanding the use of polymeric ionic liquids in headspace solid-phase microextraction: Determination of ultraviolet filters in water samples.

Science.gov (United States)

Trujillo-Rodríguez, María J; Nan, He; Anderson, Jared L

2018-03-09

Three crosslinked polymeric ionic liquid (PIL) sorbent coatings were used in headspace solid-phase microextraction for the determination of a group of ultraviolet filters. The developed crosslinked PIL-based materials include two polycations and a double confined PIL. The method, in combination with gas chromatography-mass spectrometry, is simple, solvent free, and does not require of any derivatization step. After proper optimization of the methodologies with each developed fiber, the analytical performance was compared with a commercial polyacrylate fiber. A study of the normalized calibration slopes, obtained by dividing the calibration slope of each analyte by the coating volume, revealed that the crosslinked fibers can be used as alternatives to commercial fibers for the determination of the selected group of compounds. In particular, the coating nature of the PIL containing the 1-vinylbenzyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide IL as monomer and the 1,12-di(3-vinylbenzylimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide IL as crosslinker is the most suitable for the extraction of the selected compounds despite their coating volume, being 3.6 times lower than the commercial polyacrylate fiber. For this fiber, wide linear ranges, correlation coefficients higher than 0.990, limits of detection ranging from 2.8 ng L -1 to 26 ng L -1 and relative standard deviations ranging from 2.5 to 15% were achieved. Finally, all proposed PIL-based fibers were applied towards the analysis of tap water, pool water and lake water, with the majority of the ultraviolet filters being detected and quantified in the last two types of samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Novel materials and methods for solid-phase extraction and liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

1997-06-24

This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

Determination of carbofuran on hydrophilic interaction liquid chromatography using TSK gel amide 80 as stationary phase

International Nuclear Information System (INIS)

A Kurnia; LW Lim; T Takeuchi

2016-01-01

The hydrophilic interaction liquid chromatography (HILIC) coupled to environmental friendly capillary liquid chromatography was employed to investigate retention behavior of carbofuran. Aim of this research is to investigate retention behavior of carbofuran using TSK gel amide 80 as stationary phase. Several condition was conducted to investigate retention behavior of carbofuran such as comparison study of TSK gel amide 80 with other polar column, comparison study retention behavior of carbofuran on various system wavelength, water content effect in HILIC mode, effect of buffer concentration on HILIC mode, and analytical performance. Results showed that TSK gel imidazole was superior compare to other polar stationary phase on determine carbofuran, wavelength 251 and 254 nm was resulting higher absorbance for carbofuran than others, increase of water content on mobile phase was decrease the retention time, also increase buffer salt concentration was decrease the retention time and according to analysis performance that is the accuracy was 101±10,1, the LOD 0.66 ppm while LOQ 2.22 ppm. As conclusions that TSK gel amide 80 was offering good determine on carbofuran even using capillary liquid chromatography with 10 cm length of column. (author)

Improvement of recovery and repeatability in liquid chromatography-mass spectrometry analysis of peptides

NARCIS (Netherlands)

van Midwoud, Paul M.; Rieux, Laurent; Bischoff, Rainer; Verpoorte, Elisabeth; Niederlander, Harm A. G.

2007-01-01

Poor repeatability of peak areas is a problem frequently encountered in peptide analysis with nanoLiquid Chromatography coupled on-line with Mass Spectrometry (nanoLC-MS). As a result, quantitative analysis will be seriously hampered unless the observed variability can be corrected in some way.

Gas chromatography with simultaneous detection: Ultraviolet spectroscopy, flame ionization, and mass spectrometry.

Science.gov (United States)

Gras, Ronda; Luong, Jim; Haddad, Paul R; Shellie, Robert A

2018-05-08

An effective analytical strategy was developed and implemented to exploit the synergy derived from three different detector classes for gas chromatography, namely ultraviolet spectroscopy, flame ionization, and mass spectrometry for volatile compound analysis. This strategy was achieved by successfully hyphenating a user-selectable multi-wavelength diode array detector featuring a positive temperature coefficient thermistor as an isothermal heater to a gas chromatograph. By exploiting the non-destructive nature of the diode array detector, the effluent from the detector was split to two parallel detectors; namely a quadrupole mass spectrometer and a flame ionization detector. This multi-hyphenated configuration with the use of three detectors is a powerful approach not only for selective detection enhancement but also for improvement in structural elucidation of volatile compounds where fewer fragments can be obtained or for isomeric compound analysis. With the diode array detector capable of generating high resolution gas phase spectra, the information collected provides useful confirmatory information without a total dependence on the chromatographic separation process which is based on retention time. This information-rich approach to chromatography is achieved without incurring extra analytical time, resulting in improvements in compound identification accuracy, analytical productivity, and cost. Chromatographic performance obtained from model compounds was found to be acceptable with a relative standard deviation of the retention times of less than 0.01% RSD, and a repeatability at two levels of concentration of 100 and 1000 ppm (v/v) of less than 5% (n = 10). With this configuration, correlation of data between the three detectors was simplified by having near identical retention times for the analytes studied. Copyright © 2018 Elsevier B.V. All rights reserved.

Liquid Chromatography-Tandem Mass Spectrometry: An Emerging Technology in the Toxicology Laboratory.

Science.gov (United States)

Zhang, Yan Victoria; Wei, Bin; Zhu, Yu; Zhang, Yanhua; Bluth, Martin H

2016-12-01

In the last decade, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in routine toxicology laboratories. LC-MS/MS offers significant advantages over other traditional testing, such as immunoassay and gas chromatography-mass spectrometry methodologies. Major strengths of LC-MS/MS include improvement in specificity, flexibility, and sample throughput when compared with other technologies. Here, the basic principles of LC-MS/MS technology are reviewed, followed by advantages and disadvantages of this technology compared with other traditional techniques. In addition, toxicology applications of LC-MS/MS for simultaneous detection of large panels of analytes are presented. Copyright © 2016 Elsevier Inc. All rights reserved.

Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

NARCIS (Netherlands)

Koster, E.H M; Hofman, N.S K; de Jong, G.J.

Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

Evolution and Current Trends in Liquid and Supercritical Fluid Chromatography

OpenAIRE

Fekete, Szabolcs; Grand-Guillaume-Perrenoud, Alexandre; Guillarme, Davy

2014-01-01

The current trend in high performance liquid chromatography (HPLC) tends toward the achievement of higher separation efficiency and shorter analysis time. Indeed, better performance in LC has become increasingly important in recent years mainly driven by the challenges of either analyzing more complex samples or increasing the numbers of samples per time unit. In the recent development of particle technology, the use of fully porous sub-2 m particles and sub-3 m shell particles have received ...

Experimental hydrophobicity parameters of perfluorinated alkylated substances from reversed-phase high performance liquid chromatography

NARCIS (Netherlands)

de Voogt, P.; Zurano, L.; Serné, P.; Haftka, J.J.H.

2012-01-01

Capacity factors of perfluorinated alkylated substances were obtained from isocratic reversed-phase high-performance liquid chromatography-mass spectrometry experiments at different organic modifier strengths of the mobile phase. The resulting capacity factor v. modifier strengths plots were

Determination of Urine Albumin by New Simple High-Performance Liquid Chromatography Method.

Science.gov (United States)

Klapkova, Eva; Fortova, Magdalena; Prusa, Richard; Moravcova, Libuse; Kotaska, Karel

2016-11-01

A simple high-performance liquid chromatography (HPLC) method was developed for the determination of albumin in patients' urine samples without coeluting proteins and was compared with the immunoturbidimetric determination of albumin. Urine albumin is important biomarker in diabetic patients, but part of it is immuno-nonreactive. Albumin was determined by high-performance liquid chromatography (HPLC), UV detection at 280 nm, Zorbax 300SB-C3 column. Immunoturbidimetric analysis was performed using commercial kit on automatic biochemistry analyzer COBAS INTEGRA ® 400, Roche Diagnostics GmbH, Manheim, Germany. The HLPC method was fully validated. No significant interference with other proteins (transferrin, α-1-acid glycoprotein, α-1-antichymotrypsin, antitrypsin, hemopexin) was found. The results from 301 urine samples were compared with immunochemical determination. We found a statistically significant difference between these methods (P = 0.0001, Mann-Whitney test). New simple HPLC method was developed for the determination of urine albumin without coeluting proteins. Our data indicate that the HPLC method is highly specific and more sensitive than immunoturbidimetry. © 2016 Wiley Periodicals, Inc.

Bacterial Cell Wall Precursor Phosphatase Assays Using Thin-layer Chromatography (TLC) and High Pressure Liquid Chromatography (HPLC).

Science.gov (United States)

Pazos, Manuel; Otten, Christian; Vollmer, Waldemar

2018-03-20

Peptidoglycan encases the bacterial cytoplasmic membrane to protect the cell from lysis due to the turgor. The final steps of peptidoglycan synthesis require a membrane-anchored substrate called lipid II, in which the peptidoglycan subunit is linked to the carrier lipid undecaprenol via a pyrophosphate moiety. Lipid II is the target of glycopeptide antibiotics and several antimicrobial peptides, and is degraded by 'attacking' enzymes involved in bacterial competition to induce lysis. Here we describe two protocols using thin-layer chromatography (TLC) and high pressure liquid chromatography (HPLC), respectively, to assay the digestion of lipid II by phosphatases such as Colicin M or the LXG toxin protein TelC from Streptococcus intermedius . The TLC method can also monitor the digestion of undecaprenyl (pyro)phosphate, whereas the HPLC method allows to separate the di-, mono- or unphosphorylated disaccharide pentapeptide products of lipid II.

Purification of a 166mHo solution by successive high-performance liquid chromatography and gravitational chromatography for half-life determination

International Nuclear Information System (INIS)

Florence Gueguen; Helene Isnard; Carole Bresson; Celine Caussignac; Guillaume Stadelmann; Anthony Nonell; Sebastien Mialle; Karsten Kossert; Frederic Chartier

2014-01-01

A methodology to purify a 166m Ho solution has been developed by a combination of activity and mass concentration measurements in order to further determine the 166m Ho half-life. The isobaric interference at m/q ≃ 166 requires Ho purification from non-natural Er with a high purification degree due to the large amount of Ho as opposed to Er. The Ho/Er separation was achieved using high-performance liquid chromatography on a semi-preparative column followed by purification on gravitational chromatography. The efficiency of the separation was evaluated after precise determination of the Er isotopic composition. The purification methodology enabled to separate Ho from Er. (author)

Sugar Determination in Foods with a Radially Compressed High Performance Liquid Chromatography Column.

Science.gov (United States)

Ondrus, Martin G.; And Others

1983-01-01

Advocates use of Waters Associates Radial Compression Separation System for high performance liquid chromatography. Discusses instrumentation and reagents, outlining procedure for analyzing various foods and discussing typical student data. Points out potential problems due to impurities and pump seal life. Suggests use of ribose as internal…

[Rapid determination of 8 urinary carbamate pesticides by liquid chromatography-tandem mass spectrometry].

Science.gov (United States)

Liu, Hualiang; Wang, Yuan; Zhu, Baoli

2015-11-01

To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides. After being purified by acetonitrile precipitation, urine samples were transferred to a liquid chromatography-tandem mass spectrometry system, and the concentrations of 8 carbamate pesticides were determined by external standard method. A C18 column was used for ultra-high-performance liquid chromatography; methanol/ammonium acetate solution was used as the mobile phase for gradient elution; the mass spectrometer was operated in a multi-reaction monitoring mode. The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20~800 µg/L, and the recovery rates were 61.0%~121% at spiked levels of 20, 200 and 800 µg/L, with a relative standard deviation of 1.7%~5.5%. This determination method meets the Guide for establishing occupational health standards-part 5: Determination methods of chemicals in biological materials, and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.

State-of-the art of selective detection and identification of I-, Br-, Cl-, and F-containing compounds in gas chromatography and liquid chromatography.

Science.gov (United States)

Brede, Cato; Pedersen-Bjergaard, Stig

2004-09-24

This review article presents an overview of halogen-specific detection in gas chromatography (GC) and liquid chromatography (LC). Attention is primarily focused on the use of plasma emission spectroscopy and plasma mass spectrometry as detectors, but other halogen-selective detection principles are also mentioned. Different instrumental configurations are discussed both with respect to technical set-up and performance, the principal reasons for halogen-selective detection are highlighted, and recent applications are reviewed from areas such as environmental chemistry, petroleum characterization, and drug analysis.

Activity coefficients at infinite dilution for solutes in the trioctylmethylammonium bis(trifluoromethylsulfonyl)imide ionic liquid using gas-liquid chromatography

International Nuclear Information System (INIS)

Gwala, Nobuhle V.; Deenadayalu, Nirmala; Tumba, Kaniki; Ramjugernath, Deresh

2010-01-01

The activity coefficient at infinite dilution (γ 13 ∞ ) for 30 solutes: alkanes, alkenes, cycloalkanes, alkynes, ketones, alcohols, and aromatic compounds was determined from gas-liquid chromatography (glc) measurements at three temperatures (303.15, 313.15, and 323.15) K. The ionic liquid: trioctylmethylammonium bis(trifluoromethylsulfonyl)imide, was used as the stationary phase. For each temperature, γ 13 ∞ values were determined using two columns with different mass percent packing of the ionic liquid. The selectivity (S 12 ∞ ) value was calculated from the γ 13 ∞ to determine the suitability of the solvent as a potential entrainer for extractive distillation in the separation of an hexane/benzene mixture, indicative of a typical industrial separation problem for benchmarking purposes.

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

Science.gov (United States)

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

2014-08-01

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

UV-visible scanning spectrophotometry and chemometric analysis as tools for carotenoids analysis in cassava genotypes (Manihot esculenta Crantz).

Science.gov (United States)

Moresco, Rodolfo; Uarrota, Virgílio G; Pereira, Aline; Tomazzoli, Maíra; Nunes, Eduardo da C; Martins Peruch, Luiz Augusto; Gazzola, Jussara; Costa, Christopher; Rocha, Miguel; Maraschin, Marcelo

2015-12-01

In this study, the metabolomics characterization focusing on the carotenoid composition of ten cassava (Manihot esculenta) genotypes cultivated in southern Brazil by UV-visible scanning spectrophotometry and reverse phase-high performance liquid chromatography was performed. Cassava roots rich in β-carotene are an important staple food for populations with risk of vitamin A deficiency. Cassava genotypes with high pro-vitamin A activity have been identified as a strategy to reduce the prevalence of deficiency of this vitamin. The data set was used for the construction of a descriptive model by chemometric analysis. The genotypes of yellow-fleshed roots were clustered by the higher concentrations of cis- β-carotene and lutein. Inversely, cream-fleshed roots genotypes were grouped precisely due to their lower concentrations of these pigments, as samples rich in lycopene (redfleshed) differed among the studied genotypes. The analytical approach (UV-Vis, HPLC, and chemometrics) used showed to be efficient for understanding the chemodiversity of cassava genotypes, allowing to classify them according to important features for human health and nutrition.

Graphene oxide: an adsorbent for the extraction and quantification of aflatoxins in peanuts by high-performance liquid chromatography.

Science.gov (United States)

Yu, Li; Li, Peiwu; Zhang, Qi; Zhang, Wen; Ding, Xiaoxia; Wang, Xiupin

2013-11-29

In this paper, graphene oxide (GO) was synthesized and specifically selected by centrifugation to extract four aflatoxins (B1, B2, G1, and G2) as an effective adsorbent. Then, the amount of aflatoxins was quantitatively measured by high-performance liquid chromatography (HPLC). The GO was characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), and ultraviolet (UV) spectrophotometer. Several parameters that could affect the extraction efficiency, including the GO amount, methanol concentration in the extraction solvent, spiked amount, extraction time, and elution cycle, were also investigated and optimized in this work. Under optimal conditions, good linear relationships were achieved with the correlation coefficient (r) ranging from 0.99217 to 0.99995. The detection limit of this method for the four aflatoxins ranged from 0.08 to 0.65ng/g. Finally, the proposed method has been successfully applied to determine aflatoxins in peanut samples. The results show that the recoveries of the four aflatoxins range from 85.1% to 100.8% with the relative standard deviations between 2.1% and 7.9%. Copyright © 2013 Elsevier B.V. All rights reserved.

Simultaneous analysis of FDG, ClDG and Kryptofix 2.2.2 in [18F]FDG preparation by high-performance liquid chromatography with UV detection

International Nuclear Information System (INIS)

Nakao, Ryuji; Ito, Takehito; Yamaguchi, Masatoshi; Suzuki, Kazutoshi

2008-01-01

A practical, sensitive and rapid analytical method was established and validated for chemical impurity tests of 2-deoxy-2-fluoro-D-glucose (FDG), 2-deoxy-2-chloro-D-glucose (ClDG) and Kryptofix 2.2.2 (K-222) in [ 18 F]FDG. This method was based on precolumn derivatization with ultraviolet (UV) detection. FDG and ClDG were rapidly derivatized with 1-phenyl-3-methyl-5-pyrazolone in the presence of borate buffer at 40 o C, and the labeled derivatives and K-222 were separated by reversed-phase high-performance liquid chromatography and monitored by UV absorbance at 210 nm. After optimization of the conditions, FDG, ClDG and K-222 could be determined within 15 min and showed good performance in terms of sensitivity, linearity and reproducibility. This method could be successfully applied to the quality control test of [ 18 F]FDG produced by a commercially available apparatus

Spectrophotometric determination of uranium by previous extraction chromatography separation in polimetalic mineral, phosphorites and technological licours

International Nuclear Information System (INIS)

Moreno Bermudez, J.; Cabrera Quevedo, C.; Alfonso Mendez, L.; Rodriguez Aguilera, M.

1994-01-01

The development of an analytical procedure for spectrophotometric determination of uranium in polimetalic mineral, phosphorites and technological licours is described. The method is based on the previous separation of interfering elements by extraction chromatography and on spectrophotometric determination of uranium (IV) with arsenazo III in concentrated hydrochloric acid. Tributyl phosphate impregnate on politetrafluoroethylene is used as stationary phase and 5.5 M nitric acid is used as movie phase. The influence of matrix-component elements was studies. The development procedure was applied to real samples, being the results compared with those obtained by other well established analytical methods like gamma-spectrometry, laser fluorimetric, spectrophotometry previous uranium separation by liquid liquid extraction and anion exchange. The reproducibility is evaluated and the detection limited has been established for each studied matrix. A procedure for correcting the thorium interference has been developed for samples with a Th/ 3U8O higher than 0.2

Review: Current applications and challenges for liquid chromatography coupled to isotope ratio mass spectrometry (LC/IRMS).

Science.gov (United States)

Godin, Jean-Philippe; McCullagh, James S O

2011-10-30

High-precision isotope analysis is recognized as an essential research tool in many fields of study. Until recently, continuous flow isotope ratio mass spectrometry (CF-IRMS) was available via an elemental analyzer or a gas chromatography inlet system for compound-specific analysis of light stable isotopes. In 2004, however, an interface that coupled liquid chromatography with IRMS (LC/IRMS) became commercially available for the first time. This brought the capability for new areas of application, in particular enabling compound-specific δ(13)C analysis of non-volatile, aqueous soluble, compounds from complex mixtures. The interface design brought with it several analytical constraints, however, in particular a lack of compatibility with certain types of chromatography as well as limited flow rates and mobile phase compositions. Routine LC/IRMS methods have, however, been established for measuring the δ(13)C isotopic ratios of underivatized individual compounds for application in archeology, nutrition and physiology, geochemistry, hydrology, soil science and food authenticity. Seven years after its introduction, we review the technical advances and constraints, methodological developments and new applications of liquid chromatography coupled to isotope ratio mass spectrometry. Copyright © 2011 John Wiley & Sons, Ltd.

Quantitative determination of regorafenib and its two major metabolites in human plasma with high-performance liquid chromatography and ultraviolet detection.

Science.gov (United States)

Fujita, Kazuma; Miura, Masatomo; Shibata, Hiroyuki

2016-10-01

A simple, highly sensitive and specific high-performance liquid chromatography (HPLC) method was developed for the simultaneous quantitation of regorafenib, N-oxidemetabolite (M-2) and the desmethyl N-oxide metabolite (M-5) in human plasma. Regorafenib, M-2, M-5 and the internal standard sorafenib were separated using a mobile phase of 0.5% KH2 PO4 (pH 3.5)-acetonitrile (30:70, v/v), on a Capcell PAK MG II column at a flow rate of 0.5 mL/min and measurement at UV 260 nm. The lower limits of quantification for regorafenib, M-2 and M-5 were 10 ng/mL for each analyte. A procedure using solid-phase extraction required only a small amount of plasma (100 μL) for one analysis while providing high extraction recovery (>81% for all compounds) and good selectivity. Coefficients of variation for intra- and inter-day assays were HPLC assay is suitable for clinical pharmacokinetic studies of regorafenib. The present HPLC method is currently in use for our observational studies of patients under treatment. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Characterization of phenolic compounds in Helichrysum melaleucum by high-performance liquid chromatography with on-line ultraviolet and mass spectrometry detection.

Science.gov (United States)

Gouveia, Sandra C; Castilho, Paula C

2010-07-15

Helicrysum melaleucum is a medicinal plant traditionally used in the islands of the Macaronesia region for the treatment of respiratory diseases. In this work, the phenolic compounds of Helicrysum melaleucum plants collected in different geographical locations of Madeira Island and their morphological parts (total aerial parts, leaves, flowers and stems) were extracted and analyzed separately by high-performance liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC-DAD/ESI-MS(n)). A total of 68 compounds were characterized based mainly on their UV and mass spectra. These included derivatives of O-glycosylated flavonoids (flavonol and flavones type), quinic acid, caffeic acid, lignans and polyphenols. The flowers were found to be the morphological part with higher variety of phenolic compounds. The large differences in the phenolic composition of plants collected from different geographical locations allowed the identification of a few components, such as pinoresinol and methoxylated flavone derivatives, likely to be useful as geographical markers. Also, these results promote further comparison of the bioactivities of the different samples analyzed. This paper marks the first report on the chemical analysis of Helichrysum melaleucum species. Copyright 2010 John Wiley & Sons, Ltd.

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

Science.gov (United States)

Jandera, Pavel; Hájek, Tomáš

2018-01-01

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

Sensitive determination of iodine species, including organo-iodine, for freshwater and seawater samples using high performance liquid chromatography and spectrophotometric detection

International Nuclear Information System (INIS)

Schwehr, Kathleen A.; Santschi, Peter H.

2003-01-01

In order to more effectively use iodine isotope ratios, 129 I/ 127 I, as hydrological and geochemical tracers in aquatic systems, a new high performance liquid chromatography (HPLC) method was developed for the determination of iodine speciation. The dissolved iodine species that dominate natural water systems are iodide, iodate, and organic iodine. Using this new method, iodide was determined directly by combining anion exchange chromatography and spectrophotometry. Iodate and the total of organic iodine species are determined as iodide, with minimal sample preparation, compared to existing methods. The method has been applied to quantitatively determine iodide, iodate as the difference of total inorganic iodide and iodide after reduction of the sample by NaHSO 3 , and organic iodine as the difference of total iodide (after organic decomposition by dehydrohalogenation and reduction by NaHSO 3 ) and total inorganic iodide. Analytical accuracy was tested: (1) against certified reference material, SRM 1549, powdered milk (NIST); (2) through the method of standard additions; and (3) by comparison to values of environmental waters measured independently by inductively coupled plasma mass spectrometry (ICP-MS). The method has been successfully applied to measure the concentrations of iodide species in rain, surface and ground water, estuarine and seawater samples. The detection limit was ∼1 nM (0.2 ppb), with less than 3% relative standard deviation (R.S.D.) for samples determined by standard additions to an iodide solution of 20 nM in 0.1 M NaCl. This technique is one of the few methods sensitive enough to accurately quantify stable iodine species at nanomolar concentrations in aquatic systems across a range of matrices, and to quantitatively measure organic iodine. Additionally, this method makes use of a very dilute mobile phase, and may be applied to small sample volumes without pre-column concentration or post-column reactions

Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

OpenAIRE

Preti, Raffaella

2016-01-01

The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large am...

Analysis of oak tannins by liquid chromatography-electrospray ionisation mass spectrometry.

Science.gov (United States)

Mämmelä, P; Savolainen, H; Lindroos, L; Kangas, J; Vartiainen, T

2000-09-01

Extractable tannins were analysed by liquid chromatography-electrospray ionisation mass spectrometry in two oak species, North American white oak (Quercus alba) and European red oak (Quercus robur). They mainly included various glucose gallic and ellagic acid esters. The structures were partially determined, and they included grandinin/roburin E, castalagin/vescalagin, gallic acid, valoneic acid bilactone, monogalloyl glucose, digalloyl glucose, trigalloyl glucose, ellagic acid rhamnose, quercitrin and ellagic acid.

Simultaneous quantitative analysis of metabolites using ion-pair liquid chromatography-electrospray ionization mass spectrometry

NARCIS (Netherlands)

Coulier, L.; Bas, R.; Jespersen, S.; Verheij, E.; Werf, M.J. van der; Hankemeier, T.

2006-01-01

We have developed an analytical method, consisting of ion-pair liquid chromatography coupled to electrospray ionization mass spectrometry (IP-LC-ESI-MS), for the simultaneous quantitative analysis of several key classes of polar metabolites, like nucleotides, coenzyme A esters, sugar nucleotides,

Simultaneous determination of seven anticoagulant rodenticides in agricultural products by gel permeation chromatography and liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Saito-Shida, Shizuka; Nemoto, Satoru; Matsuda, Rieko; Akiyama, Hiroshi

2016-11-01

A sensitive and reliable method for the simultaneous determination of hydroxycoumarin-type (brodifacoum, bromadiolone, coumatetralyl, and warfarin) and indandione-type (chlorophacinone, diphacinone, and pindone) rodenticides in agricultural products by gel permeation chromatography (GPC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The procedure involved extraction of the rodenticides from samples with acetone, followed by liquid-liquid partitioning with hexane/ethyl acetate (1:1, v/v) and 10% sodium chloride aqueous solution, then cleanup using GPC, and finally, analysis using LC-MS/MS. High recoveries from the GPC column were obtained for all rodenticides tested using a mobile phase of acetone/cyclohexane/triethylamine (400:1600:1, v/v/v). An ODS column, which contains low levels of metal impurities, gave satisfactory peak shapes for both hydroxycoumarin- and indandione-type rodenticides in the LC-MS/MS separation. The average recoveries of rodenticides from eight agricultural foods (apple, eggplant, cabbage, orange, potato, tomato, brown rice, and soybean) fortified at 0.0005-0.001 mg/kg ranged from 76 to 116%, except for bromadiolone in orange (53%) and diphacinone in soybean (54%), and the relative standard deviations ranged from 1 to 16%. The proposed method effectively removed interfering components, such as pigments and lipids, and showed high selectivity. In addition, the matrix effects were negligible for most of the rodenticide/food combinations. The results suggest that the proposed method is reliable and suitable for determining hydroxycoumarin- and indandione-type rodenticides in agricultural products.

Determination of atenolol in human plasma using ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography.

Science.gov (United States)

Zeeb, Mohsen; Farahani, Hadi; Papan, Mohammad Kazem

2016-06-01

An efficient analytical method called ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography was developed for the determination of atenolol in human plasma. A hydrophobic ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was formed by the addition of a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate) to a sample solution containing an ion-pairing agent during microextraction. The analyte was extracted into the ionic liquid phase while the microextraction solvent was dispersed throughout the sample by utilizing ultrasound. The sample was then centrifuged, and the extracting phase retracted into the microsyringe and injected to liquid chromatography. After optimization, the calibration curve showed linearity in the range of 2-750 ng/mL with the regression coefficient corresponding to 0.998. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.5 and 2 ng/mL, respectively. A reasonable relative recovery range of 90-96.7% and satisfactory intra-assay (4.8-5.1%, n = 6) and interassay (5.0-5.6%, n = 9) precision along with a substantial sample clean-up demonstrated good performance of the procedure. It was applied for the determination of atenolol in human plasma after oral administration and some pharmacokinetic data were obtained. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Derivative spectrophotometry of cobalt alloys

International Nuclear Information System (INIS)

Spitsyn, P.K.

1985-01-01

The method of derivative spectrophotometry is briefly described, and derivative absorption spectra are presented for samarium, cobalt, and commercial Sm-Co alloys. It is shown that the use of derivative spectrophotometry not only improves the accuracy and selectivity of element determinations but also simplifies the analysis of alloys. Results of a statistical evaluation of the metrological characteristics of the analytical procedure described here are presented. 8 references

Analytical method by high resolution liquid chromatography for the determination of carbamazepine in human plasma

International Nuclear Information System (INIS)

Jimenez Aleman, Narda M; Calero Carbonell, Jorge E; Padron Yaquis, Alejandro S; Izquierdo Lozano, Julio C

2007-01-01

One of the requirements to develop the studies of bioavailability and bioequivalence is to have analytic methodologies validated for the work with samples in biological fluids. A method was developed by high resolution liquid chromatography for the determination of carbamazepine in human plasma. A mixture of hydrogen phosphate of sodium: acetonitrile (65:35) adjusted to pH= 3.3 with phosphoric acid, flow of 1.2 mL/min and ultraviolet detection at 210 nm, was used as mobile phase. Propylparabene was used as an internal standard. According to the established regulations for the validation of the methods in biological fluids, the following parameters were studied: stability of the samples, lineality, specificity, precision, accuracy and limit of detection and quantification. The method proved to be specific and sensitive with a detection and quantification limit of 0.9 and 1.0 ng, respectively. The method was lineal, precise and exact in the range of concentrations of 1. 07 at 12.67 μg/mL. The mean recovery was not statistically different from 100.0 %. The analito in the proposed biological matrix remained in the studied period. The methodology described in this work is applied in our case to the study that evaluates the bioavailability and bioequivalence of a Cuban formulation of carbamazepine in healthy volunteers. (Author)

Determination of Aspartame, Caffeine, Saccharin, and Benzoic Acid in Beverages by High Performance Liquid Chromatography.

Science.gov (United States)

Delaney, Michael F.; And Others

1985-01-01

Describes a simple and reliable new quantitative analysis experiment using liquid chromatography for the determinaiton of caffeine, saccharin, and sodium benzoate in beverages. Background information, procedures used, and typical results obtained are provided. (JN)

Modern Aspects Of Fluorometric Detection In Liquid-Phase Chromatography

Science.gov (United States)

Bousquet, Bernard; Garnier, Jean P.; Dreux, Claude

1983-10-01

Recent advances are described in the combined use of fluorometric derivatization and high performance liquid chromatography (HPLC) for clinical chemistry determinations. Derivatives (especially dansyl derivatives) can be formed prior to chromatography in the case of estrogens, amino acids, and catecholamines. In post-column reactions, we preferred to use air-segmented reactions as they conform better to all the optimized chromatographic and spectrofluorometric parameters. Fluorescent derivatives produced from cate-cholamines, tryptophan and its metabolites, hydroxyindoles, tryptamine, amino acids, sugars, polyamines, and other substances are often sufficiently sensitive to be detected in picogram quantities by HPLC. Their reaction principle and some of their applications to samples are described. Recently, chemical excitation of fluorophore-like dansyl amino acid was proposed as a detection system for HPLC. By a post-column reaction, a fluorophore can be made to emit light by its reaction with trichlorophenyl oxalate (TCPO) and hydrogen peroxide. The detection limit of this system is about 10 fmol for each dansyl amino acid. Application of this new reaction to catecholamines opens up new prospects for fluorometric detection.

Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

Science.gov (United States)

Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

2016-03-18

Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

Alternative sample-introduction technique to avoid breakthrough in gradient-elution liquid chromatography of polymers

NARCIS (Netherlands)

Reingruber, E.; Bedani, F.; Buchberger, W.; Schoenmakers, P.

2010-01-01

Gradient-elution liquid chromatography (GELC) is a powerful tool for the characterization of synthetic polymers. However, gradient-elution chromatograms often suffer from breakthrough phenomena. Breakthrough can be averted by using a sample solvent as weak as the mobile phase. However, this approach