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At least 19 recordsLinked to original sources
PubMed1989

High performance liquid chromatographic determination of diclofenac sodium in plasma using column-switching technique for sample clean-up.

For routine analysis of diclofenac sodium in plasma, a new high performance liquid chromatographic method, which is combined with column-switching technique is developed. The precolumn packed with Corasil RP C-18 was connected to analytical column by switching system in order to enrich the sample drugs in plasma without extraction. This method showed excellent sensitivity, precision and reproducibility. The limit of detection, using a 100 microL injection of plasma, was 0.1 micrograms/mL and the mean coefficient of variation for intra- and inter-assay was better than 4.6%. Total analysis time was 20 min between injections. The present method offers distinct practical advantages over conventional liquid-liquid extraction methods of sample preparation with respect to time, effort, recovery, and sample volume required. The method has been applied to the samples from rats receiving oral administration of diclofenac sodium.

Chromatography, High Pressure Liquid↗
PubMedDate not supplied

Simple and highly sensitive determination of free fatty acids in human serum by high performance liquid chromatography with fluorescence detection.

A highly sensitive and simple reversed phase high performance liquid chromatographic (HPLC) method for the quantitative determination of free fatty acids in human serum is presented. The method is based on the direct derivatization of serum fatty acids with 6,7-dimethoxy-1-methyl-2(1H)-quinoxalinone-3-propionylcarboxylic acid hydrazide. The derivatization reaction proceeds in aqueous solution in the presence of pyridine and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide at 37 degrees C. The resulting derivatives are separated within 75 min on a reversed phase column (YMC Pack C8) with a gradient elution of aqueous acetonitrile and detected fluorimetrically. The detection limits are 2.5-5 fmol in a 10 microL injection volume. The sensitivity permits precise determination of free fatty acids in 5 microL serum. The method is simple and is without the conventional liquid-liquid extraction steps of serum fatty acids.

Chromatography, High Pressure Liquid↗
PubMed1988

Optimization of the quantitative analysis of the major cannabis metabolite (11-nor-9-COOH-delta 9-tetrahydrocannabinol) in urine by gas chromatography/mass spectrometry.

A gas chromatographic/mass spectrometric electron impact method is presented for the detection and quantification of 11-nor-9-carboxy-delta 9-tetrahydrocannabinol (THC-COOH) in urine, for use in the confirmation of presumptive results obtained by other techniques. Four extraction procedures, two solid-liquid and two liquid-liquid, have been compared. A comparison of two trimethylsilylating methods demonstrates that the best results are obtained by the use of a mixture containing N-methyl-N-trimethylsilyl-trifluoroacetamide, trimethyliodosilane and dithioerithritol (100:0.2:1) v/v/w. The use of ketoprofen as a new internal standard for the quantification of THC-COOH has proved to be very effective. Both spiked samples and samples from cannabis users have been successfully analysed. It has also been demonstrated that the presence of other drugs of abuse in urine samples do not interfere with cannabis quantification by the method reported here.

Dronabinol↗
PubMed1990

High-performance liquid chromatography/tandem mass spectrometry: its use for the identification of stanozolol and its major metabolites in human and equine urine.

A screening procedure for the anabolic steroid stanozolol in human and equine urine was developed based on enzymatic hydrolysis, liquid-liquid extraction and reversed-phase liquid chromatography combined on-line with tandem mass spectrometry. The column effluent was introduced into the atmospheric pressure ionization source of a triple-quadrupole mass spectrometer via a heated pneumatic nebulizer liquid chromatograph/mass spectrometer interface. Abundant protonated molecular ions were generated by corona discharge ionization. Confirmation of stanozolol and several of its hydroxylated and dihydroxylated metabolites isolated from both human and equine urine was accomplished by collision-induced dissociation of their parent ions. Interpretation of the daughter ion mass spectra gave valuable information for the structural elucidation of the detected metabolites. Using the selected reaction monitoring detection mode the presence of the urinary excretion products could be monitored in equine urine up to one day and in human urine for several days after oral administration of stanozolol. Microbore high-performance liquid chromatography/ion spray mass spectrometry of an ion-pair extract enabled the direct detection of intact sulfoconjugated hydroxy-metabolites in human urine.

Animals↗
PubMed1991

Determination of the antidepressant levoprotiline and its N-desmethyl metabolite in biological fluids by gas chromatography/mass spectrometry.

A specific and sensitive gas chromatographic/mass spectrometric method was developed and validated for the determination of the antidepressant levoprotiline in blood, plasma and urine and the simultaneous determination of levoprotiline and its desmethyl metabolite in urine. Deuterium-labelled analogues were used as internal standards. The compounds were isolated from the biological fluids by liquid-liquid extraction under basic conditions. Following derivatization with perfluoropropionic anhydride, the samples were analysed by capillary column gas chromatography/electron impact mass spectrometry with selected ion monitoring. The analysis of spiked samples demonstrated the high accuracy and precision of the method. Blood concentrations of levoprotiline down to 0.7 nmol l-1 (1 ml used for analysis) could be quantified with a coefficient of variation of 10% or less. The method is suitable for use in pharmacokinetic and bioavailability studies of levoprotiline in humans.

Antidepressive Agents↗
PubMed1992

Validation of a gas chromatographic/mass spectrometric method for the determination of (E)-beta-fluoromethylene-m-tyrosine and its active metabolite in human plasma and urine.

(E)-beta-Fluoromethylene-m-tyrosine (FMMT, MDL 72394) represents a prodrug approach to site-selective, irreversible inhibition of monoamine oxidase. A sensitive and specific method for the quantification of FMMT and its active metabolite (MDL 72392) in human plasma and urine has been developed for future pharmacokinetic studies. The procedure consists of a liquid-liquid extraction of plasma and urine samples, esterification with HCl/butanol and, subsequently, N-acylation with pentafluoropropionic anhydride. This is followed by gas chromatography/mass spectrometry employing negative ion chemical ionization. The precision and the accuracy of the method have been optimized by using two internal standards: MDL 72661 (a methyl homologue of FMMT) for the quantification of FMMT, and MDL 72761 (a methyl homologue of MDL 72392) for the quantification of MDL 72392. The method has been validated for FMMT and MDL 72392 over the concentration range 2.5-400 pmol ml-1 with a limit of quantification for both compounds of 2.5 pmol ml-1. Sample clean-up and selected ion monitoring by mass spectrometry ensured the specificity and sensitivity required for the pharmacokinetic evaluation of FMMT and MDL 72392.

Gas Chromatography-Mass Spectrometry↗
PubMed1990

High-performance liquid chromatographic resolution of oxamniquine enantiomers: application to in vitro metabolism studies.

A method is described for the HPLC analysis of oxamniquine enantiomers in liver fraction incubates, using a second-generation alpha 1-acid glycoprotein-based column (Chiral-AGP). Oxamniquine is extracted from the incubation media by liquid-liquid extraction, using diethyl ether. The dried residue is redissolved in eluent, filtered, then injected directly onto the analytical column. The extraction method affords recoveries of oxamniquine of approximately 93%, at concentrations up to 525 micrograms/ml, with an average relative standard deviation of 5.9%. The limit of detection of the method (to give an SNR = 2 at 246 nm) is 0.3 ng on-column for the first eluting, laevorotatory enantiomer and 2.3 ng for the dextrorotatory isomer. The method allowed study of the depletion of oxamniquine enantiomers in liver postmicrosomal incubates. In the rat, a turnover of 21.9% was observed, with no apparent enantioselectivity. Similar observations were made for a mouse liver subcellular fraction incubation. The absence of enantioselectivity in this biotransformation may be attributable to the low substrate specificity of the oxidase or dehydrogenase enzymes involved.

Animals↗
PubMed1992

Plasma determination of the enantiomers of SL 84.0418, a new antihyperglycaemic drug, by HPLC on a chiral alpha 1-AGP column.

SL 84.0418 is a new antihyperglycaemic drug. It is an orally active and selective alpha 2-adrenoceptor antagonist. This molecule, a pyrroloindole derivative, contains an asymmetric center yielding two enantiomers. In order to evaluate the pharmacokinetic profile of both enantiomers following oral administration of the racemate we have developed an HPLC method for their separation and quantification. The liquid-liquid extraction involved three steps with two salting-out procedures at pH 11.5 before and after a back-extraction with 0.005 M H2SO4. The enantiomers were separated by HPLC on a stainless-steel column (100 x 4.0 mm) packed with a chiral alpha 1-acid. The UV response was linear from 1 to 250 ng/ml for both enantiomers. The relative standard deviation (RSD) for reproducibility was below 10.7%. Using quality control samples, precision was found below 7.8% and accuracy was 108%. Extraction recoveries were ca. 60% for both enantiomers and 94% for the internal standard. Column life was brought up to 2 months, which corresponds to about 1,000 injections of biological extract. No guard column was used, but a daily back-flush was carried out. This method is suitable for routine analysis and 30 to 40 plasma samples a day can be processed. This method allows the definition of the pharmacokinetic profile of both enantiomers of SL 84.0418 in human plasma after single oral administration of doses as low as 20 mg of the racemic drug.

Adrenergic alpha-Antagonists↗
PubMed1990

Electrically enhanced extraction of penicillin G into dichloromethane.

The application of electrically enhanced liquid-liquid extraction techniques to the recovery and purification of penicillin G from aqueous solutions and from untreated mycelial culture broth is described. Experiments at laboratory scale have shown that extraction rates into dichloromethane at pH 4.0 may be increased by factors of up to five-fold by electrostatically spraying penicillin G solutions into a continuum of solvent held in electrical tension. The experimental studies revealed that in small spray column contactors, electrostatic spray conditions, once initiated at nozzle voltages in excess of 10 kV, could be sustained at nozzle voltages as little as 4 kV. The results demonstrate the potential of this technique as an alternative to mechanically augmented liquid-liquid contact for the intensification of whole broth extraction processes.

Biotechnology↗
PubMed1977

High-performance liquid chromatographic determination of diethylpropion hydrochloride in tablets: isolation and identification of two decomposition products.

A rapid assay was developed for diethylpropion hydrochloride tablets using high-performance liquid chromatography (HPLC) with UV detection. This technique provided separation of the drug from other UV-absorbing components present as the result of decomposition. A major decomposition product detected by HPLC in extracts of tablets and of the cotton filler from a tablet bottle was collected from the column effluents. This product was subsequently identified as 1-phenyl-1,2-propanedione, a highly volatile compound. A second decomposition product, isolated from decomposed drug by distillation from alkaline solution, was identified as diethylamine, apparently present as the hydrochloride salt, GLC, UV, IR, NMR, and mass spectrometry were used to confirm the identity of the decomposition products. HPLC assay results compared favorably with results of the NF assay; the latter procedure separated the drug from 1-phenyl-1,2-propanedione via liquid-liquid extraction.

Chromatography, Gas↗
PubMed1979

Improved method for morphine extraction from biological samples.

Methadone morphine, or naloxone extraction from brain homogenates, plasma, and urine is described. An aqueous sample was loaded on a surgical gauze support, which was washed with extracting solvents. Aqueous samples remained on the support, and nonpolar drugs partitioned into the lipophilic extracting solvent. The procedure recovered 80-100% of nanogram levels of methadone, morphine, or naloxone from biological samples. In addition, an approximate 10-fold timesaving capacity was demonstrated compared to standard liquid-liquid extraction techniques.

Animals↗
PubMed1979

High-performance liquid chromatographic microdetermination of indoprofen in human milk.

A previously reported high-performance liquid chromatographic (HPLC) method for indoprofen determination in physiological fluids was modified and extended to provide quantitative data on drug concentrations in human milk samples at a low nanogram per milliliter level. The reversed-phase HPLC technique was modified to give a better separation of the drug and milk components. To achieve the necessary cleanup for low level determination, the milk samples required protein precipitation, liquid-liquid drug extraction, and concentration. Excellent indoprofen recovery was obtained with this technique; the average recovery from 20 milk samples spiked with various nanogram drug levels was 95%. The analytical technique showed excellent reproducibility; the calibration solutions over 15 days had a relative standard deviation of 3.2%. Results for indoprofen levels in milk and plasma samples from seven subjects who received either a single or multiple oral drug dose are presented.

Chromatography, High Pressure Liquid↗
PubMed1985

Liquid chromatographic assay for fluoxymesterone in human serum with application to a preliminary bioavailability study.

Fluoxymesterone was extracted from serum with a liquid-liquid extraction procedure. Serum containing both drug and internal standard, 6 alpha-methylprednisolone, was extracted with methylene chloride. The extract was washed with 0.1 M NaOH and water, evaporated, and reconstituted with mobile phase. Chromatography was performed on a Zorbax Sil column, preceded by a guard column, with a mobile phase composed of 50% water-saturated butyl chloride:tetrahydrofuran:methanol:phosphoric acid (880:100:15:0.5). Fluoxymesterone and methylprednisolone were detected by UV absorption at 236 nm. Overall recovery was 80%. Calibration curves were linear for fluoxymesterone concentrations from 5 to 100 ng/mL. The assay is accurate and precise (RSD values less than or equal to 7%); endogenous steroids did not interfere with the assay. Assay suitability was assessed in a bioavailability study in which six subjects each received two treatments of 10-mg fluoxymesterone tablets in a Latin-square crossover study. The two treatments were a tablet administered either buccally or orally. Cmax values ranged from 40 to 150 ng/mL with tmax values of 1-2 h. The harmonic mean half-life of fluoxymesterone was 2.0 h. Less than 8% of the AUC was extrapolated. Mean Cmax and AUC values from the oral treatment were 80 and 76%, respectively, of the mean values from the buccal treatment.

Adult↗
PubMed1987

Stereoselective determination of (beta S,gamma R and beta R,gamma S)-4-[3-(4-acetyl-3-hydroxy-2-propylphenoxy) propylthio]-gamma-hydroxy-beta-methylbenzenebutanoic acid in human and rat plasma by normal-phase high-performance liquid chromatography.

A stereoselective high-performance liquid chromatographic method was developed for the determination of the enantiomeric composition comprising (beta S,gamma R and beta R,gamma S)-4-[3-(4-acetyl-3-hydroxy-2-propylphenoxy) propylthio]-gamma-hydroxy-beta-methylbenzenebutanoic acid in human and rat plasma. Both enantiomers, (beta S,gamma R)- and (beta R,gamma S)-1, were isolated from the plasma by liquid-liquid extraction, the organic phase was evaporated to dryness, and the residue was lactonized with p-toluenesulfonic acid followed by derivatization with R(+)-alpha-methylbenzylamine to form diastereomeric Schiff base adducts. Separation was performed on a silica column (Supelcosil) with a mobile phase composed of 97.8% hexane, 2% isopropyl alcohol, and 0.2% triethylamine. The column eluant was monitored with a variable wavelength UV detector set at 280 nm (0.005 AUFS). Based on the peak area ratios, the method shows excellent linear relationships with their corresponding concentrations and satisfactory intraday and interday assay precision and accuracy. The detection limit of this method is 25 ng/mL in plasma for each enantiomer. The method has been applied to the assay of plasma obtained from human subjects administered 1 in safety and tolerability studies and from rats administered 1 intravenously or per os.

Animals↗
PubMed1989

Automated robotic extraction and subsequent analysis of diclofenac in plasma samples.

Diclofenac sodium (Voltaren;sodium[O-(2,6-dichloroanilino)phenyl]acetate), an effective, well-tolerated anti-inflammatory agent, is almost completely metabolized in humans and animals. The present article describes an automated procedure involving liquid-liquid extraction and subsequent HPLC analysis to determine unchanged diclofenac in human plasma. This procedure offers several advantages over current manual GC and HPLC methods. The transfer of the original manual procedure to an automated robotic system, with custom-made modules for solvent evaporation and HPLC injection, is described, and a comparison between the manual and automated procedure is drawn. The robotic method gave satisfactory accuracy and precision in the range of 0.02 to 3 micrograms/mL, with a quantitation limit of 0.02 micrograms/mL.

Autoanalysis↗
PubMed1990

Stereoselective determination of flecainide in human plasma by high-performance liquid chromatography with fluorescence detection.

Enantiomers of a drug may differ in their pharmacological activities or their disposition constants. We now describe a stereoselective analytical method for the determination of the antiarrhythmic agent flecainide in plasma. The resolution of the enantiomers is achieved by high-performance liquid chromatography (HPLC) on a normal phase silica column following derivatization with the optically active reagent (-)-methyl chloroformate. The eluting diastereoisomers are monitored by fluorescence detection at an excitation wavelength of 305 nm and an emission wavelength of 340 nm. The limit of sensitivity for the assay is as low as 2.5 ng/mL for each enantiomer using 1 mL of plasma. A new liquid-liquid extraction procedure with high recovery (greater than 95%) and high selectivity is also reported. The intra- and interassay coefficient of variation for replicated analysis of spiked plasma samples is less than 4.0% and 7.0%, respectively. The method is suitable for single and multiple dose pharmacokinetic studies in healthy volunteers or in patients.

Chromatography, High Pressure Liquid↗
PubMed1990

Determination of iloprost in 5% dextrose in water solution by reversed-phase high performance liquid chromatography.

A high-performance liquid chromatographic (HPLC) method utilizing absorbance detection was developed for the rapid and precise determination of the stable prostacyclin analogue iloprost in 5% dextrose in water solution (D5W). Samples were prepared for chromatographic analysis by extracting the drug into chloroform, evaporating the solvent, and solubilizing the residue in methanol. The resulting solutions were chromatographed on a Shandon ODS Hypersil column using 0.02 M potassium phosphate (pH 3.0), methanol, and acetonitrile (456:144:400, v/v) at a flow rate of 1.8 mL/min. 2-Naphthoic acid was employed as an internal standard. The detector response at 207 nm was linear (correlation coefficient greater than 0.9998) for concentrations of iloprost from 10 ng on-column, the lower limit of quantitation, up to 7 micrograms on-column. The precision of the method was approximately 5% based on peak area, with a recovery of iloprost from D5W of 87%. Liquid-liquid extraction was found to be superior to solid-phase sorbent extraction as a sample preparation method due to incompatibility of dextrose with the sorbent bed.

Chemical Phenomena↗
PubMed1992

Separation and quantitation of polyethylene glycols 400 and 3350 from human urine by high-performance liquid chromatography.

Polyethylene glycol 3350 (PEG 3350) is useful as an orally administered probe to measure in vivo intestinal permeability to macromolecules. Previous methods to detect polyethylene glycol (PEG) excreted in the urine have been hampered by inherent inaccuracies associated with liquid-liquid extraction and turbidimetric analysis. For accurate quantitation by previous methods, radioactive labels were required. This paper describes a method to separate and quantitate PEG 3350 and PEG 400 in human urine that is independent of radioactive labels and is accurate in clinical practice. The method uses sized regenerated cellulose membranes and mixed ion-exchange resin for sample preparation and high-performance liquid chromatography with refractive index detection for analysis. The 24-h excretion for normal individuals after an oral dose of 40 g of PEG 3350 and 5 g of PEG 400 was 0.12 +/- 0.04% of the original dose of PEG 3350 and 26.3 +/- 5.1% of the original dose of PEG 400.

Adult↗