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PubMedDate not supplied

A routine HPLC method for monitoring midazolam in serum.

A routine high-performance liquid chromatographic method for measuring midazolam in human serum has been developed. The sample preparation procedure consisted of simple liquid-liquid extraction with dichloromethane, followed by evaporation under nitrogen. The mobile phase used was a mixture of acetonitrile at 0.02 M and sodium acetate at pH 3.0 (80:20, v/v) and a flow-rate of 1.2 mL/min. The separation was performed on two cyanopropyl columns (150 x 4.6 mm). The detection was by UV absorption at 240 nm. A linear range from 10 to 1,000 ng/mL and a quantification limit of 7.4 ng/mL of serum was reached. The mean intra-assay and inter-assay reproducibility from serum sample spiked with 100 ng/mL were 4.1 and 4.7%, respectively. The recoveries from serum sample spiked with 50, 100, 500 ng/mL were 85.46, 85.38 and 85.57%, respectively. This method was developed to allow pharmacokinetics study of midazolam in young patients in short surgical interventions.

Chromatography, High Pressure Liquid↗

PubMedDate not supplied

Simple method for simultaneous determination of halothane, enflurane, and isoflurane in Krebs solution using capillary gas chromatography.

A simple gas chromatography (GC) method for the simultaneous determination of halothane, enflurane, and isoflurane in Krebs buffer solution has been developed. The method utilizes methylene chloride as the internal standard and liquid-liquid extraction using chloroform as the solvent. The method demonstrated excellent recovery (100%) of each component and a linear calibration range of 100-700, 100-800, and 300-1,400 micrograms/mL for halothane, isoflurane, and enflurane, respectively. Intra-day accuracy and precision had an error and coefficient of variation of less than 5.1% and 2.7%, respectively.

Anesthetics, Inhalation↗

PubMedDate not supplied

High sensitivity determination of the remoxipride hydroquinone metabolite NCQ-344 in plasma by coupled column reversed-phase liquid chromatography and electrochemical detection.

An HPLC method for the determination of NCQ-344, a remoxipride metabolite with a hydroquinone structure, in human plasma is described. Special precautions for the sampling were necessary as the compound rapidly decomposes. An efficient clean-up of the plasma samples was necessary to make use of the inherent sensitivity of the electrochemical detector. This was accomplished by a fast and simple liquid-liquid extraction at pH 7.05 combined with further cleaning on-line by using a short cyanopropyl column as the first column in a column switching system. A heart-cut from the cyanopropyl column containing the NCQ-344 fraction was then injected onto the analytical octadecyl silica column and NCQ-344 was detected at an oxidation potential of 0.70 V. The absolute recovery was > 95% and concentrations down to 0.10 nM could be determined with acceptable precision. The NCQ-344 levels in a limited number of samples from patients given remoxipride were found to be between 0.10 and 1 nM. The remoxipride concentrations in the same samples were 5,000-20,000 nM.

Chromatography, High Pressure Liquid↗

PubMed1999

Quantitative determination of clenbuterol enantiomers in human plasma by high-performance liquid chromatography using the macrocyclic antibiotic chiral stationary phase teicoplanin.

We report a method for the high-performance liquid chromatographic (HPLC) chiral separation of racemic clenbuterol in human plasma. Human plasma was spiked with stock solutions of clenbuterol hydrochloride and practolol as the internal standard. Following a liquid-liquid extraction procedure with 10% (+/-)-2-butanol/isopropyl ether under alkaline conditions, the dried samples were reconstituted in methanol and chromatographed using a macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T(trade mark) (teicoplanin). The mobile phase composition was methanol:acetonitrile (70:30, v/v), containing 0.3% (v/v) acetic acid and 0.2% (v/v) triethylamine. The resulting chromatogram achieved baseline separation for the clenbuterol enantiomers. Calibration curves (peak area ratio vs plasma concentration, n = 10) were constructed for the (-)-R-and (+)-S-clenbuterol enantiomers with a plasma concentration range of 0. 25-10 microM. The correlation coefficient (r) range was 0.99988-0. 99999 (mean = 0.99999). The lowest concentration measured was 0.25 microM. Inter- and intra-assay variation was determined for the lowest, medium and highest plasma concentration (0.25, 2 and 10 microM) by calculating the analytical recoveries with a range of 96-104%. The percentage recoveries for the clenbuterol enantiomers were 88.4-102% over the concentration range used. Detailed methodology is presented.

Chromatography, High Pressure Liquid↗

PubMed1999

An antiviral furanoquinone from Paulownia tomentosa Steud.

A methanol extract of the stem bark of Paulownia tomentosa showed antiviral activity against poliovirus types 1 and 3. Sequential liquid-liquid extraction with n-hexane, chloroform and water, and a silicagel column chromatography resulted in the purification of a compound. The compound was identified as methyl-5-hydroxy-dinaphthol[1,2-2',3']furan-7,12-dione-6-carbox yla te on the basis of spectroscopic data. The component caused a significant reduction of viral cytopathic effect when it was subjected to a standard antiviral assay by using HeLa cells. The EC(50) of the compound against poliovirus type 1 strain Brunhilde, and type 3 strain Leon were 0.3 microg/mL and 0.6 microg/mL, respectively.

Antiviral Agents↗

PubMed1997

Enantioselective high-performance liquid chromatography assay of (+)R- and (-)S-alpha-lipoic acid in human plasma.

A specific plasma level assay for the enantiomers of alpha-lipoic acid is described. It makes use of liquid-liquid extraction, chemical reduction to the dithiol enantiomers, and their precolumn chiral derivatisation with o-phthalaldehyde in the presence of D-phenylalanine. The two diastereomeric derivatives are separated by reversed-phase HPLC with fluorescence detection. The working range of the assay is between 15 ng/ml (lower limit of quantitation) and 1,000 ng/ml for either enantiomer.

Calibration↗

PubMed1999

Development of validated stereoselective methods for methadone determination in clinical samples.

A stereoselective analysis of methadone (Mtd) in whole blood and serum was developed using liquid chromatography on a protein based chiral stationary phase. Liquid-liquid extraction (LLE) and solid phase extraction methods were applied before chromatographic analysis. The extraction procedure, as well as the choice of the biological matrix, showed significant differences in the extraction yield and in the precision of the assays. Serum was selected for this assay and LLE was chosen as the preparation step because of its simplicity and rapidity. The total procedure was validated and applied to clinical samples. Samples taken from 45 heroin-addicted patients were analyzed. A correlation was found between the dose administered and Mtd concentration (total and R-form), but interindividual variability of the total normalized Mtd was seen (concentration varied from 90 to 530 ng/ml). Furthermore, two populations were apparently observed with a mean Mtd concentration of 200 and 475 ng/ml, respectively. Stereoselective analyses showed that more than 50% of the patients presented a nonracemic ratio, and particularly about 25% showed a preferential metabolism of the active R-Mtd enantiomer. Therefore, the stereoselective determination of Mtd is necessary to improve the quality of the treatment of heroin addiction.

Chromatography, Liquid↗

PubMed1999

Achiral and chiral determination of tramadol and its metabolites in urine by capillary electrophoresis.

An achiral and chiral separation for the determination of tramadol and its main metabolite O-demethyltramadol in urine samples by CE with UV detection was developed. It was possible to separate tramadol and its phase I and phase II metabolites in one single run using a borate buffer. Furthermore, the simultaneous chiral separation of tramadol and the phase I metabolites was achieved using carboxymethyl-beta-cyclodextrin as chiral selector. To reach the required limits of quantification for the analytes, a preconcentration by solid-phase extraction for the achiral assay and by liquid-liquid extraction for the chiral assay was used. The methods were validated and their applicability was shown by the determination of tramadol and O-demethyltramadol in urine samples.

Analgesics, Opioid↗

PubMed2000

Coupling of solvent semimicroextraction with capillary electrophoresis using ethyl acetate as sample matrix.

This paper reports a strategy to couple liquid-liquid semimicroextraction (LLsME) with capillary electrophoresis (CE) based on a newly introduced on-column decomposable sample matrix, ethyl acetate (EA). LLsME was performed in volumetric flasks of 100 mL. Samples containing an aqueous phase were first saturated with EA. Then, an extra 500 microL of EA was added to extract the samples. Sample injection in CE could be made in hydrodynamic mode by dipping the injection end of the capillary into the organic (EA) phase in the volumetric flasks. As a demonstration, alkylphenones in water samples were extracted by LLsME into EA and subjected to separation by micellar electrokinetic chromatography (MEKC). Alkylphenones of C8-C12 with concentrations of about 10 ppb can be concentrated and detected after extraction; extraction efficiencies range from 72- to 334-fold. Linearity of extraction was determined and the effect on reproducibility by spiking an internal standard was studied. The method developed is time-saving and requires no further special experimental device other than a basic CE setup. Therefore, it would be readily acceptable for routine analysis, especially in analytical laboratories dealing with environmental samples.

Acetates↗

PubMed2000

Gas chromatography/negative ion chemical ionization mass spectrometry and liquid chromatography/electrospray ionization tandem mass spectrometry quantitative profiling of N-acetylcysteine conjugates of valproic acid in urine: application in drug metabolism studies in humans.

We report a GC/NICI-MS assay and a LC/ESI-MS/MS assay for the analysis of N-acetylcysteine (NAC) conjugates of (E)-2,4-diene VPA (NAC I and NAC II) identified in humans. The assay also includes the analysis of the NAC conjugate of 4,5-epoxy VPA (NAC III), an identified metabolite in rats treated with 4-ene VPA for its use in metabolic studies in animals. The highly sensitive GC/MS assay was designed to monitor selectively the diagnostic and most abundant [M - 181](-) fragment anion of the di-PFB derivatives of NAC I, NAC II, and NAC IV, the internal standard (IS) and the PFB derivative of NAC III. The higher selectivity of LC/MS/MS methodology was the basis for an assay which could identify and quantitate the underivatized conjugates simultaneously using MRM of the diagnostic ions m/z 130 and 123 arising from the CID of their protonated molecular ions [MH](+). The GC/MS assay employed liquid-liquid extraction whereas the LC/MS/MS assay used a solid-phase extraction procedure. Linearity ranges of the calibration curves were 0.10-5.0microg ml(-1) by GC/MS and 0.10-1.0microg ml(-1) by LC/MS/MS for NAC I, NAC II and NAC III (r(2) = 0.999 or better). Both assays were validated for NAC I and NAC II and provided good inter- and intra-assay precision and accuracy for NAC I and NAC II. The LOQ by LC/MS/MS was 0.1microg ml(-1), representing 1 ng of NAC I and NAC II. The same LOQ (0.1microg ml(-1)) was observed by GC/MS and was equivalent to 100 pg of each metabolite. NAC III was detected at concentrations as low as 0.01 microg ml(-1) by both methods. The total urinary excretion of the NAC conjugates in four patients on VPA therapy was determined to be 0.004-0.088% of a VPA dose by GC/MS and 0.004-0. 109% of a VPA dose by LC/MS/MS.

Acetylcysteine↗

PubMed2000

Quantitation of simvastatin and its beta-hydroxy acid in human plasma by liquid-liquid cartridge extraction and liquid chromatography/tandem mass spectrometry.

A sensitive and reliable procedure for the simultaneous determination of simvastatin (SV) and its active beta-hydroxy acid metabolite (SVA) in human plasma was developed and validated. The analytes were extracted simultaneously from 0.5 ml aliquots of human plasma samples by methyl tert-butyl ether (MTBE) via Chem Elut cartridge extraction [also called liquid-solid extraction (LSE) or liquid-liquid cartridge extraction (LLCE)], separated through a Kromasil C(18) column (50 x 2 mm i.d. 5 microm) and detected by tandem mass spectrometry with a turbo ionspray interface. Stable isotope-labeled SV and SVA, (13)CD(3)-SV and (13)CD(3)-SVA, were used as internal standards. SV and SVA were detected in positive and negative ion modes, respectively, via within-run polarity switching. The use of Chem Elut cartridges not only provided a simple and efficient means of plasma sample extraction but also successfully reduced the interconversion between SV and SVA to an undetectable (for lactonization of SVA) or negligible (<0.07%, for hydrolysis of SV) level. The method showed excellent reproducibility, with intra- and inter-assay precisions <4.5% (RSD), and intra- and inter-assay accuracy between 94% and 107% of nominal values, for both analytes. The extraction recoveries were 78% and 87% on average for SV and SVA, respectively. The analyte was found to be stable in plasma through three freeze (-70 degrees C)-thaw (4 degrees C) cycles and for at least 3 h under bench-top storage condition in an ice-bath (4 degrees C), and also in the reconstitution solution at 4 degrees C for at least 24 h. The method has a lower limit of quantitation (LOQ) of 50 pg ml(-1) with a linear calibration range of 0.05-50 ng ml(-1) for both analytes, and has proved to be very reliable for the analysis of clinical samples.

Anticholesteremic Agents↗

PubMed2000

Determination of brain and plasma drug concentrations by liquid chromatography/tandem mass spectrometry.

A method is described for the evaluation of drug concentrations in plasma and brain from treated rats. The analyte is recovered from plasma or brain homogenate by liquid-liquid extraction and subsequently analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). A simple experimental protocol renders the procedure valuable for obtaining information rapidly on brain penetration and plasma exposure of specific classes of compounds. This methodology has been applied to evaluate brain penetration with 30 different compounds from the same discovery program. In an attempt to increase throughput in our screening efforts, mixture dosing was evaluated. Results from single compound administration were compared with results following administration of a mixture of four compounds. Preliminary results, with specific classes of compounds, show no major differences (ranking order) in brain or plasma concentrations between mixture dosing and single compound administration, suggesting that mixture dosing could be applicable to brain penetration studies in the drug discovery phase.

Animals↗

PubMed2000

Characterization of zirconium complexes of interest in spent nuclear fuel reprocessing by electrospray ionization mass spectrometry

Liquid-liquid extraction of zirconium, one of the most important fission products, was followed using electrospray ionization mass spectrometry under conditions simulating reprocessing of nuclear spent fuel. Zr(IV) can precipitate from the organic phase after extraction by dibutylphosphoric acid (HDBP), the most common degradation product of tributylphosphate (TBP) radiolysis. Different complexes were detected with electrospray used in positive or negative ion modes, according to the extraction conditions such as the ligand/metal ratio. Stoichiometry of the Zr(IV) complexes was determined by combining isotopic labeling [H(15)NO(3)] of the aqueous phase in the extraction system and tandem mass spectrometry experiments. These results were compared with the species observed using other techniques reported in the literature. The mechanisms of ionization/desorption of these complexes are proposed depending on the organic ligand character (neutral (L) such as TBP, or acidic (HL') such as HDBP), and the ionization mode used. Copyright 2000 John Wiley & Sons, Ltd.

Journal Article↗

PubMed2001

Validation of liquid-liquid extraction followed by flow-injection negative ion electrospray mass spectrometry assay to Topiramate in human plasma.

This paper describes the development and validation of a method for the quantitative analysis of Topiramate (2,3:4,5-bis-O-(1-methylethylidene)-beta-D-fructopyranose sulfamate), a new antiepileptic drug, in human plasma using liquid-liquid extraction followed by flow-injection negative ion electrospray mass spectrometry. Using Prednisone (1,4-pregnadiene-17-alpha,21-diol-3,11,20-trione [10 microg/mL]) as an internal standard, calibration curves for Topiramate were linear over a range of 1 to 30 microg/mL in human plasma and were highly reliable (r(2) = 0.9991). The lower limit of quantitation of the assay was 2 microg/mL in human plasma. Precision (%CV <15%) and accuracy (<20%) for both intra- and inter-day validations were satisfactory. The method has been used in clinical pharmacology research.

Anticonvulsants↗

PubMed2000

A novel high-pressure liquid-liquid extraction process for downstream processing in biotechnology: extraction of cardiac glycosides.

This investigation examines phase equilibrium phenomena that can be used to create two water-like solvents for liquid-liquid extraction in downstream processing in biotechnology: a completely miscible, binary liquid mixture of water and a hydrophilic organic solvent (e. g., an alcohol) reveals a liquid phase split, when it is pressurized with a "near-critical" gas (i.e., a substance which at ambient conditions is a gas, near its critical temperature). This phase split results in two hydrophilic liquid phases. Making use of this phenomenon in process development first requires research on the phase split phenomenon and, second, research on the feasibility of biomolecule extraction and separation. In this study, basic fluid phase equilibrium phenomena are briefly described. Then, experimental results are reported for the partitioning of small amounts of cardiac glycosides (digitoxin and digoxin) on coexisting liquid phases in the high-pressure, three-phase, vapor-liquid-liquid equilibrium of the ternary system of "near critical" CO(2) + water + 1-propanol, at 313 K and 333 K. Finally, a process for extraction and separation of the aforementioned glycosides by means of the high-pressure phase equilibrium phenomenon is discussed.

1-Propanol↗

PubMed2000

Enhancement of mass transfer using colloidal liquid aphrons: measurement of mass transfer coefficients in liquid-liquid extraction.

Interphase mass transfer of a sparingly soluble solute is often the rate-limiting step in multiphase biocatalytic processes. Colloidal liquid aphrons (CLA) provide very large interfacial areas, and thus could enhance mass transfer in such processes. The aim of this study was to characterize mass transfer properties of CLA dispersions during transfer of heptanoic acid from water to limonene. The interfacial area per unit volume (a), film mass transfer coefficient (K(L)), and volumetric mass transfer coefficient (K(L)a) values were determined in a stirred-tank reactor. These results were used, along with a literature correlation, to estimate the mass transfer coefficient of the surfactant-stabilized shell surrounding the CLA. The very large increase in a provided by the CLA was only partially offset by a slight increase in the mass transfer resistance of the shell. As a result, the range of K(L)a values obtained using CLA was about an order of magnitude greater than that obtained using a conventional dispersion. The concentration of the aqueous-phase surfactant used to form the CLA strongly affected the Sauter mean diameter of the CLA; however, the concentration of the nonpolar-phase surfactant had little effect. These results suggest that CLA have considerable potential for multiphase biocatalytic applications.

Biotechnology↗

PubMed2000

High-performance liquid chromatographic determination of naltrexone in plasma of hemodialysis patients.

A simple, sensitive, selective and reliable reversed-phase high-performance liquid chromatographic (HPLC) method with UV detection is described for the determination of naltrexone in plasma samples. Naltrexone and the internal standard, naloxone, were isolated from plasma either with a liquid-liquid extraction method using ethyl acetate or with a solid-phase extraction method using Sep-Pack C18 cartridge before chromatography. The extracts were dried under a stream of nitrogen and the samples were reconstituted in the mobile phase, then 20 microL were injected on a Waters Symmetry C18 column (5 microm particle size, 4.6 x 150 mm). The mobile phase consisted of 0.06% triethylamine (pH 2.8)-acetonitrile (92:8, v/v) pumped at 1 mL/min. The peak-area ratio versus plasma concentration was linear over the range of 10-500 ng/mL and the detection limit was less than 8 ng/mL. Quantification was by ultra-violet detection at 204 nm. The present method was applied to the determination of the plasma concentration of naltrexone in dialyzed patients. Patients (n = 8) with severe generalized pruritus received 50 mg of naltrexone orally per day for 2 weeks. The variability in the therapeutic response in treated patients required plasma concentration investigations of this opioid antagonist.

Chromatography, High Pressure Liquid↗

PubMed2000

Enantioselective determination of bromoisovalerylurea by liquid chromatography on chiral stationary phase in reversed- or normal-phase partition mode.

Bromoisovalerylurea (bromvalerylurea) is a sedative-hypnotic given orally as a racemate. Enantiomers of this drug could be separated by high-performance liquid chromatography on the three chiral stationary phases (a vancomycin-bonded, beta-cyclodextrin derivative-bonded, or urea derivative-bonded phase). Biological fluids of human subjects who had ingested toxic or therapeutic doses of the racemate were chromatographed after liquid-liquid extraction. The (+)-enantiomer concentration was almost equal to the (-)-enantiomer concentration in the serum of one overdosed patient. In all the other subjects, the (+)-enantiomer was less than the (-)-enantiomer in their sera and saliva. The data suggest that the drug is absorbed non-stereoselectively from the gastrointestinal tract and eliminated from the blood stereoselectively.

Adult↗