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At least 19 recordsLinked to original sources
PubMed1982

Midazolam determination by gas chromatography, liquid chromatography and gas chromatography--mass spectrometry.

Midazolam is determined in serum by gas chromatography with a nitrogen-selective detector, by liquid chromatography, and by gas chromatography--mass spectrometry. Comparable results are obtained with the three techniques with a within-run precision of 9% by gas chromatography and gas chromatography---mass spectrometry and 5% by liquid chromatography. Between-run precision is 13% by gas chromatography--mass spectrometry and 10% by liquid chromatography. Comparison of patient's sera by gas chromatography (x), liquid chromatography (y), and by gas chromatography (x), gas chromatography--mass spectrometry (y) gave correlations of 0.98 and 0.89, respectively. Interferences observed when using one technique, for example liquid chromatography, can be eliminated by analyzing the sample extract with one of the other techniques.

Anti-Anxiety Agents↗
PubMed2000

Analysis of anthocyanins in foods by liquid chromatography, liquid chromatography-mass spectrometry and capillary electrophoresis.

This article reviews recent developments in the methodology for the measurement of anthocyanins that offer several advantages over classical methods of analysis. The use of UV-diode array and mass spectrometric (MS) detectors, with improved methods of liquid chromatography analysis has facilitated identification of these analytes. The use of capillary electrophoresis (CE) analysis of the anthocyanins under acid conditions has significantly increased peak resolution and improved the detection limits by several orders of magnitude. CE offers the advantage of economies of very small sample size, very small solvent consumption, and short analysis times along with the future possibility of being combined with MS detection.

Anthocyanins↗
PubMed1978

Comparative determination of phenytoin by spectrophotometry, gas chromatography, liquid chromatography, enzyme immunoassay, and radioimmunoassay.

Sera from patients being treated with phenytoin were analyzed for the drug by spectrophotometry, gas chromatography, radioimmunoassay, enzyme immunoassay, and liquid chromatography. The essay values obtained were intercompared statistically. Enzyme immunoassay and liquid chromatography appear to be attractive alternatives to the more traditional methods of spectrophotometry and gas chromatography. Our radioimmunoassay data correlated poorly with results by the four other methods.

Chromatography, Gas↗
PubMed1980

A comparison of serum phenytoin determination by the substrate-labeled fluorescent immunoassay with gas chromatography, liquid chromatography, radioimmunoassay and "EMIT".

Patients' sera were analyzed for phenytoin by the Substrate-Labeled Fluorescent Immunoassay (SLFIA), gas chromatography (GC), liquid chromatography (LC), Radioimmunoassay (RIA) and EMIT and the results were compared. The EMIT assay was performed using a "PACER Analyzer". All assay results compared favorably. The correlation coefficients were: SLFIA vs GC, 0.995 (n = 45); SLFIA vs. LC, 0.993 (n = 37); SLFIA vs. EMIT, 0.965 (n = 67); SLFIA vs. RIA, 0.977 (n = 34). These results show that phenytoin levels determined by the SLFIA compare well with those obtained by the other four assay techniques.

Chromatography, Gas↗
PubMed1979

Disopyramide determination by gas chromatography, liquid chromatography, and gas chromatography--mass spectrometry.

Disopyramide is determined in serum by gas chromatography with a nitrogen-selective detector, by liquid chromatography, and by gas chromatography--mass spectrometry. Comparable results are obtained with the three techniques, with a within-run and between-run precision of 5 to 10% (coefficient of variation). Least-squares analysis of data on patients' sera, analyzed first by gas chromatography (y) and then liquid chromatography (x), gave a slope of 1.12; y-intercept, -0.31; standard error of estimate, 0.46; and correlation coefficient, 0.94. Comparison of patients' sera by gas chromatography (y) and then by gas chromatography--mass spectrometry (x) gave a slope of 0.94; y-intercept, 0.42; standard error of estimate, 0.38; and correlation coefficient, 0.97. Interferences observed when using one technique--for example, gas chromatography--can be eliminated by analyzing the sample extract with one of the other techniques.

Chromatography, Gas↗
PubMedDate not supplied

Comparison of micellar electrokinetic chromatography, liquid chromatography, and microbiologic assay for analysis of cephalexin in oral suspensions.

Two well-accepted methodologies, based on a microbiologic assay (MA) and liquid chromatography (LC), and a novel methodology using micellar electrokinetic chromatography (MEKC), were compared for the determination of cephalexin in commercially available and simulated samples of oral suspensions. The MA, described in the Brazilian Pharmacopeia, was performed with a strain of Staphylococcus aureus ATCC 6538 as the test organism, following the cylinder-plate method. The LC analysis followed the European Pharmacopoeia, 3rd Ed., and was used with minor modifications. The MEKC analysis was based on a previous work of the group. Estimates of the repeatability relative standard deviations of the MA, LC, and MEKC methods in the analysis of a commercial sample were 0.34, 0.42, and 0.37%, respectively. The recovery obtained with LC was 99.90 +/- 1.11%; for MEKC, it was 100.09 +/- 0.56%. Although the 3 methodologies were statistically equivalent for the determination of cephalexin in oral suspensions, MA gave suitable repeatability despite being nonspecific and time-consuming. MEKC provided faster analysis and higher column efficiency, whereas LC presented superior sensitivity. The results indicated that MEKC can be used as an alternative method to MA and LC in routine quality control laboratories.

Anti-Bacterial Agents↗
PubMed1999

Analysis of 9-fluorenylmethyloxycarbonyl derivatives of catecholamines by high performance liquid chromatography, liquid chromatography/mass spectrometry and tandem mass spectrometry.

9-Fluorenylmethyloxycarbonyl (FMOC) derivatives of catecholamines, including dopamine (DA; 3,4-dihydroxyphenethylamine), norepinephrine (NE; 2-amino-1-(3,4-dihydroxyphenyl)ethanol) and epinephrine (EPI; 1-phenyl-1-hydroxy-2-methylaminopropane) as well as 3, 4-dihydroxybenzylamine (DHBA) have been analyzed using high performance liquid chromatography coupled to fluorometric detection and atmospheric pressure chemical ionization mass spectrometry at low femtomole levels. Structures of the derivatives have also been characterized by liquid chromatography/atmospheric pressure chemical ionization mass spectrometry and electrospray/tandem mass spectrometry. Protonated molecules of FMOC-DA and FMOC-DHBA as well as [M + H - H(2)O](+) ions of FMOC-NE and FMOC-EPI appear in their conventional mass spectra, and abundant fragments characteristic of catecholamines dominated the spectra. Structurally diagnostic ions using several hundred femtomoles of the FMOC derivatives of catecholamine were observed. Collision-induced dissociation (CID) of electrospray-generated protonated molecules of FMOC-DA and FMOC-DHBA as well as [M + H - H(2)O](+) ions of FMOC-NE and FMOC-EPI produced diagnostic product ion spectra. Liquid chromatography/atmospheric pressure chemical ionization mass spectrometric analysis of the FMOC derivatives of catecholamines and DHBA should prove useful in the separation and characterization of these compounds from biological materials.

Animals↗
PubMed2000

Determination of the metabolites of gestrinone in human urine by high performance liquid chromatography, liquid chromatography/mass spectrometry and gas chromatography/mass spectrometry.

Gestrinone was studied by high performance liquid chromatography (HPLC) for screening and by gas chromatography/mass spectrometry (GC/MS) for confirmation. When the chromatograms of blank, spiked urine and dosed urine were compared by HPLC, two unknown metabolites were found and these were excreted as the conjugated forms. Metabolites 1 and 2 were tested by LC/MS and LC/MS/MS and both had parent ions at m/z 325. The fragment ion of metabolite 1 was at m/z 263 and ions for metabolite 2 were m/z 307 [MH - H(2)O](+), 289, 279 and 241. LC/MS/MS of m/z 263 as the parent ion of metabolite 1 gave fragment ions at m/z 245 and 217, which were assumed to be [263 - H(2)O](+) and [235 - H(2)O](+), respectively. The trimethylsilyl (TMS)-enol-TMS ether derivative of gestrinone displayed three peaks in its GC/MS chromatogram, formed by tautomerism.

Adult↗
PubMed1977

Gas-liquid chromatography and liquid chromatography of ethylenethiourea in fresh vegetable crops, fruits, milk, and cooked foods.

The Onley-Yip procedure for determining ethylenethiourea (ETU) in milk and crops was modified to reduce interferences by the ethylenebisdithiocarbamates (EBDCs). A 20 g crop-methanol extract is cleaned up by adsorbing the sample onto Gas-Chrom S. desorbing ETU, and eluting ETU from aluminum oxide with chloroform containing ethanol. ETU is converted to the S-butyl derivative for gas-liquid chromatography (GLC) and flame photometric detection (sulfur mode). For liquid chromatography (LC), ETU is cleaned up on another aluminum oxide column and injected directly. LC and GLC results are confirmed by thin layer chromatography. A cooking procedure based on conversion of EBDCs to ETU is included for surveying crops for possible EBDC content. Recoveries from 8 crops and milk fortified at 0.05 ppm ETU ranged from 73 to 100%.

Animals↗
PubMed2005

Strategy for metabonomics research based on high-performance liquid chromatography and liquid chromatography coupled with tandem mass spectrometry.

Metabonomics, the study of metabolites and their roles in various disease states, is a novel methodology arising from the post-genomics era. This methodology has been applied in many fields. Current metabonomic practice has relied on mass spectrometry (MS), gas chromatography-mass spectrometry (GC-MS), and nuclear magnetic resonance (NMR) to analyze metabolites. In this study, a strategy was developed for applying high-performance liquid chromatography (HPLC) and LC-MS-MS to metabonomics research. One of the key problems to be solved in this strategy is to match the peaks between the chromatograms. A peak alignment algorithm has been developed to match the chromatograms before the pattern recognition. As an application example, the strategy described above was applied to metabonomics research on liver diseases, and the false-positive result of live cancer diagnosis from the hepatocirrhosis and hepatitis diseases was effectively reduced to 7.40%. Based on the pattern recognition, several potential biomarkers were found and further identified by the following LC-MS-MS experiments. The structures of eight potential biomarkers were given for distinguishing the liver cancer from the hepatocirrhosis and hepatitis diseases.

Adult↗
PubMed2004

Determination of malachite green residues in rainbow trout muscle with liquid chromatography and liquid chromatography coupled with tandem mass spectrometry.

A method for the determination of malachite green and its major metabolite leucomalachite green in rainbow trout muscle is reported with limits of detection of 0.8 and 0.6 microg kg(-1), respectively. Residues were extracted with an acetonitrile-acetate buffer mixture and partitioned into methylene chloride. Clean-up of the extracts was performed on alumina and propylsulfonic acid solid-phase extraction columns using the automated solid-phase extraction system. The chromatographic separation of malachite green and leucomalachite green was achieved on a Chromspher 5B column using an acetonitrile-acetate buffer mobile phase. Leucomalachite green was converted to malachite green by post-column oxidation before spectrophotometric detection at 600 nm. The mean recoveries of malachite green and leucomalachite green from control rainbow trout muscle spiked at 2-50 microg kg(-1) were 65% (range 63.4-65.9%, relative standard deviation 3.9-16.1%) and 74% (range 58.3-82.6%, relative standard deviation 3.3-11.4%), respectively. Qualitative confirmation of the determined residues was performed with liquid chromatography coupled with tandem mass spectrometry detection with limits of detection of 2.5 and 1 microg kg(-1) for malachite green and leucomalachite green, respectively.

Aniline Compounds↗
PubMed1988

Comparison of the chromatographic properties of sterols, select additional steroids and triterpenoids: gravity-flow column liquid chromatography, thin-layer chromatography, gas-liquid chromatography and high-performance liquid chromatography.

The chromatographic properties of approximately 100 sterols, select steroids of plant origin (sapogenins and steroidal alkaloids) and triterpenoids has been evaluated in this laboratory by monitoring their elution characteristics in adsorption (gravity column and thin-layer methods with and without the addition of silver nitrates), gas and reversed-phase high-performance liquid chromatography. The utility of each methodology to act in one or another chromatographic mode-separation, radio-chemical purification, quantitation and structural elucidation, is discussed. The importance of the tilt of the -OH group at C-3 as well as the polarity, size, an shape of the rest of the molecule as it effects the hydrogen-bonding ability of the -OH group is demonstrated through changes in chromatographic behavior that result from the step-wise introduction of double bonds, methyl, bromo, oxygen, nitrogen and cyclopropyl groups into 5 alpha-cholestanol. An independent aid in the structure identification and quantitation of the compounds was use of a multiple-wavelength diode array detector in which different wavelengths of the UV spectrum (200-400 nm) were simultaneously monitored following passage of the sample through a reversed-phase C18 column.

Chromatography, Gas↗
PubMed2002

Determination of water-soluble UV-filters in sunscreen sprays by liquid chromatography.

Liquid chromatography was used for the determination of the three most used water-soluble UV filters, benzophenone-4 (BZ4), terephthalylidene dicamphor sulfonic acid (TDS), and phenylbenzimidazole sulphonic acid (PBS), in aqueous sunscreen sprays. A C18 stationary phase and an isocratic mobile phase of EtOH-20 mM sodium acetate buffer of pH 4.6 (30:70, v/v) were used at a flow-rate of 0.5 ml min(-1). Mobile phase was also used as solvent for samples and standards. UV detection was at 313 nm. The analytical run took 5.5 min. The limits of detection were 0.5, 0.9 and 2 microg ml(-1) for BZ4, TDS and PBS, respectively. The proposed method does not involve highly toxicsolvents.

Chromatography, Liquid↗
PubMedDate not supplied

Overloaded hollow-fiber liquid chromatography.

Liquid chromatography in hollow fibers can separate solutes like flavors and proteins by using a stationary phase of organic solvent, sometimes containing reversed micelles. Such separations, which have a much smaller pressure drop than equivalent separations in packed beds, show dispersion consistent with chromatographic theories at low flows and dilute feeds. These separations behave less predictably at high flows and concentrated feeds, which overload the hollow fibers. The results for flavors correlate well with the Graetz number, consistent with available theories of chromatography and adsorption. The results for proteins correlate poorly with the Graetz number but better with a dimensionless flux based on facilitated diffusion in the stationary phase.

Absorption↗
PubMedDate not supplied

Investigation of the kinetics of degradation of hexopyranosylated cytosine nucleosides using liquid chromatography.

Liquid chromatography was used to follow the degradation of hexopyranosylated cytosine nucleosides in buffers of acid, neutral and alkaline pH and of constant ionic strength. The compounds were found to degrade by hydrolysis to cytosine and/or by deamination to the corresponding uracil nucleosides. Degradation in acid is influenced by the number of sugar hydroxyl groups, presence of sugar double bonds and the type of anomer. Stability of some of the compounds was compared with that of related thymine nucleosides. Temperature studies support a unimolecular mechanism of hydrolysis at pH 1.22.

Buffers↗
PubMedDate not supplied

Stored wheat insect infestation related to uric acid as determined by liquid chromatography.

Liquid chromatography is used to measure the uric acid content of wheat internally infested by various growth stages of granary weevil (Sitophilus granarius), rice weevil (Sitophilus oryzae), and lesser grain borer (Ryzopertha dominica). Good correlation exists between numbers of insects and uric acid content of grain infested by a given stage of an internally infesting stored product insect, with correlation coefficients ranging from 0.970 to 0.998. Uric acid content of infested grain increases as the insect life cycle progresses, with granary weevil producing the greatest quantities of uric acid followed in order by rice weevil and lesser grain borer. A detection limit for the analytical procedure of less than 1.0 ppm uric acid allows detection of infestation levels as low as one kernel per 100 g grain for late instar granary weevil larvae. This limit is sufficiently sensitive to detect levels of infestation that may be commonly encountered in commerce.

Animals↗
PubMed2004

[Study on thermostability and photo-isomerization of trans-resveratrol by high performance liquid chromatography and liquid chromatography-electrospray ionization-mass spectrometry].

The thermostability and photo-isomerization reaction mechanism of trans-resveratrol were studied by using high performance liquid chromatography (HPLC) and liquid chromatography-electrospray ionization-mass spectrometry ( LC-ESI-MS). A reversed-phase Hypersil-ODS column was used with the mobile phase consisting of 60/40 methanol-water, with addition of 0.05% trifluoroacetic acid for HPLC, and 0.1% formic acid and 5 mmol/L ammonium formate for LC-ESI-MS, at a flow rate of 0.5 mL/min. Diode array detection was set at 300 nm and the injection volume was 20 or 10 microL. Mass spectrometric conditions were in the negative mode. The results of thermostability test under 4, 20 and 40 degrees C indicated that the concentration of trans-resveratrol, after storage for 600 h, was decreased slightly under 4 degrees C, decreased by 5% under 20 degrees C, and 10% under 40 degrees C. In addition, the photo-isomerization reaction of trans- and cis-resveratrol under 254 nm and 365 nm UV irradiation was investigated by LC-ESI-MS, showing that the isomerization is based on p-status, and that some secondary reactions are radical induced.

Chromatography, High Pressure Liquid↗
PubMed2002

Chromatographic screening for zopiclone and metabolites in urine using liquid chromatography and liquid chromatography-mass spectrometry techniques.

Zopiclone is a benzodiazepine-like hypnotic that was believed not to have any abuse potential. Nevertheless, during the past few years there have been an increasing number of reports on the abuse and misuse of zopiclone. Despite this, methods for screening analysis in urine are lacking. To investigate whether UV detection would be possible to use for this purpose, a liquid chromatography method with ultraviolet detection for analyzing zopiclone and its urinary metabolites was developed, with liquid chromatography-mass spectrometry for confirmation. The method was used for analyzing samples from subjects receiving methadone. The limits of detection were approximately 100 ng/mL in control urine samples and 500 ng/mL in urine samples from subjects receiving methadone. However, due to the high background in these patients' urine, a single therapeutic dose was impossible to detect.

Adult↗