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At least 1,621 records · Page 90Linked to original sources
PubMed1999

Monitoring of zonisamide in human breast milk and maternal plasma by solid-phase extraction HPLC method.

An HPLC method was developed for the determination of zonisamide in human breast milk and plasma. Chromatographic separation was achieved using a Develosil CN analytical column with potassium dihydrogenphosphate buffer (pH 3.5 with milk, pH 2.5 with plasma)-acetonitrile as the mobile phase. Zonisamide and 1, 2-benzisoxazole-3-methansulfonamine acetate as internal standard were detected by ultraviolet absorbance at 240 nm. Zonisamide in breast milk and plasma was extracted by a rapid and simple procedure based on C(18) bonded-phase extraction. Determination of zonisamide in human breast milk and plasma was possible in the concentration range 0.05-20.0 microg/mL. The recoveries of zonisamide added to human breast milk and plasma were 79.5-85.0% and 86.3-93.1%, respectively, with coefficients of variation of less than 8.3% and 11.4% respectively. The mean concentrations of zonisamide in breast milk and plasma were 9.41 +/- 0.95 and 10.13 +/- 0.45 microg/mL, respectively. The average ratio between the breast milk concentration and plasma concentration (M/P ratio) was 0.93 +/- 0.09.

Adult↗
PubMed1999

Multi-residue analysis of N-methylcarbamate pesticides and their hydrolytic metabolites in environmental waters by use of solid-phase extraction and micellar electrokinetic chromatography.

A method for the simultaneous separation and determination of N-methylcarbamate pesticides and their hydrolytic metabolites by micellar electrokinetic chromatography (MEKC) was developed. A mixture of five pesticides (carbaryl, propuxur, carbofuran, aminocarb, and methiocarb) and their corresponding phenols was studied to optimize the separation of its components in terms of various electrophoretic parameters such as buffer type, pH and concentration, sodium dodecyl sulfate concentration, injection conditions, and applied voltage. Excellent separation of all ten analytes was achieved within about 20 min. The optimized method was used for determinations in environmental water samples. Sample volumes of 250 mL were first preconcentrated in the pesticides and metabolites by passage through a LiChrolut EN sorbent column and then further enriched by on-column stacking. Dynamic ranges of 40 ng/L - 6 microg/L, limits of detection at the nanogram-per-liter level, and relative standard deviations from 2.6 to 7.4% were obtained. The proposed method surpasses high-performance liquid chromatography (HPLC) in separation efficiency. In fact, it provides more expeditious separations and allows more flexible adjustment of the selectivity. Also, it enables the quantification for the analytes studied in this work with decreased limits of detection.

Carbamates↗
PubMed1986

Solid phase extraction and isocratic separation of urinary porphyrins by HPLC.

A method for determining urine porphyrins by HPLC is described. In the preliminary step, porphyrins are purified in high yields and concentrated by low pressure reverse-phase chromatography on C18 (octadecylsilane bonded silica) cartridge. Porphyrins are stable for 10 days after adsorption on C18 cartridge. The separation of porphyrin esters is performed on an aminopropyl-bonded silica column with an eluting system containing n-heptane and ethyl acetate. The system enables rapid isocratic separation of porphyrin methyl esters with high selectivity. The simplicity and reproducibility of the whole procedure allows its application to the routine analysis of urinary porphyrins in the clinical laboratory.

Chromatography, High Pressure Liquid↗
PubMed1987

Determination of 4-methylpyrazole in plasma using solid phase extraction and HPLC.

A rapid method for the determination of 4-methylpyrazole in plasma is described. Internal standard (3-methylpyrazole) is added to the plasma which is subsequently applied to a BondElut SCX column. After washing the column the 3- and 4-methylpyrazoles are eluted with a phosphate buffer and analyzed by isocratic reversed-phase high performance liquid chromatography with UV detection. The concentration of 4-methylpyrazole is calculated from the 4-methylpyrazole/3-methylpyrazole peak height ratio. The method is linear between 2.5 and 100 mumol/L with a within-day precision (CV) of 2.2% (n = 10) and a day-to-day precision of 2.8% (n = 30). The sensitivity is sufficient for analysis of plasma levels in the low micromolar range.

Chromatography, High Pressure Liquid↗
PubMed1989

Solid phase extraction and HPLC determination of spiramycin in plasma and vitreous concentrations.

A method for extracting spiramycin by an octadecylsilica cartridge is described for plasma or vitreous samples. The macrolide antibiotic is then measured by reversed-phase HPLC with UV detection. The limit of detection is estimated to be 50 ng/mL. The coefficient of variation for the procedure is 6.1% and 5.2% for the range of concentrations 0.2 micrograms/mL and 10 micrograms/mL respectively. By this method, pharmacokinetic profiles were performed for five adult patients. Spiramycin could be accurately measured in the vitreous humour, allowing the determination of antibiotic at its site of action.

Chromatography, High Pressure Liquid↗
PubMed1989

Determination of halofuginone in bovine plasma by competing-ion high performance liquid chromatography after solid phase extraction.

A high performance liquid chromatography (HPLC) method for the determination of the anticoccidial and antitheilerial drug halofuginone in bovine plasma was developed. Samples were diluted with acetic acid (10%, v/v) and cleaned up on a Bond Elut C8 column. The analyte was eluted from the extraction column and chromatographed by reversed-phase HPLC using decylamine as a competing-ion reagent. Detection was by UV at 243 nm. Recovery from plasma was 75%, and within-day and between-day coefficients of variation were 5.23 and 6.35% respectively. The specificity and sensitivity of this method (limit of detection in plasma, 1 ng/mL) were sufficiently high to enable us to characterize the time course of the drug in plasma after oral administration of therapeutic doses to cattle.

Administration, Oral↗
PubMed1990

Solid phase extraction and high performance liquid chromatographic determination of doxophylline in plasma.

A sensitive and selective high performance liquid chromatographic doxophylline assay with ultraviolet detection has been developed for plasma samples. The drug is isolated from biological samples with a reversed phase C18 disposable extraction column. Plasma standard curves are linear for concentrations of doxophylline from 0.03 to 10 mg/L. At the therapeutic range concentrations, the recoveries are better than 96.9%. The coefficients of variation for the procedure are 4.1% and 2.7% for the concentrations 0.03 mg/L and 10 mg/L, respectively. By this method, pharmacokinetic profiles are obtained for six adult volunteers.

Adult↗
PubMed1991

Determination of short-chain fatty acids in equine caecal liquor by ion exchange high performance liquid chromatography after solid phase extraction.

A high performance liquid chromatography (HPLC) method was developed for the determination of seven short-chain fatty acids in equine caecal liquor. Samples were cleaned up on a Sep-pak (C18) cartridge, and the analyte was eluted from the extraction cartridge and filtered through a 0.45 micron cellulose nitrate filter. The analyte was chromatographed by ion exchange HPLC. Detection was by UV at 210 nm. Recovery from phosphate buffer (0.05 M, pH 7.0) and equine caecal liquor was 76.95% (lactic), 76.76% (valeric). The limit of (propionic), 89.35% (isobutyric), 88.73% (butyric), 80.33% (isovaleric) and 72.61% (valeric). The limit of detection of the short-chain fatty acids in phosphate buffer was 0.00006 M (lactic), 0.0001 M (acetic), 0.0002 M (propionic), 0.0001 M (isobutyric), 0.0002 M (butyric), 0.0002 M (isovaleric) and 0.0003 M (valeric). The specificity and sensitivity of this method was sufficiently high to allow the characterization of the pattern of these short-chain fatty acids in equine caecal liquor following intravenous administration of oxytetracycline at the recommended dose rate in a pony.

Animals↗
PubMed1991

Solid phase extraction of oxcarbazepine and its metabolites from plasma for analysis by high performance liquid chromatography.

A rapid, sensitive and simple-to-operate high performance liquid chromatographic method for the simulataneous determination of oxcarbazepine, 10-hydroxycarbazepine and 10,11-dihydro-10,11-trans-dihydroxy-carbamazepine in plasma is described. The drug and its metabolites were extracted from plasma using commercially available reversed phase octadecylsilane bonded-silica columns (Bond Elut C18, 1 mL capacity). Chromatographic separation of oxcarbazepine and its metabolites was achieved using a mobile phase consisting of acetonitrile/methanol/water (13:25:62 by volume) at a flow rate of 1.2 mL/min in conjunction with a Waters Associates Nova-Pak C18 column. The analytical column, in Radial-Pak cartridge form, was used in combination with a LiChrospher 5 microns C18 guard column. By measuring the UV absorbance at 214 nm, plasma levels in the region of 50-100 ng/mL for the drug and its metabolites can be detected with only 100 microL of plasma. The method has been applied to pharmacokinetic studies of oxcarbazepine and its metabolites in children with epilepsy; preliminary pharmacokinetic findings in two patients at steady-state are presented.

Anticonvulsants↗
PubMedDate not supplied

Analysis of morphine and its 3- and 6-glucuronides by high performance liquid chromatography with fluorimetric detection following solid phase extraction from neonatal plasma.

A rapid, sensitive and simple to operate high performance liquid chromatographic method for the simultaneous determination of morphine, morphine-3-glucuronide and morphine-6-glucuronide in plasma is described. The drug and its metabolites were extracted from plasma using commercially available reversed phase octylsilane bonded silica columns (1 mL Bond Elut C8, 50 mg). Chromatographic separation of morphine and its metabolites was achieved using a mobile phase, consisting of 2 mM sodium dodecyl sulphate in 0.05% phosphoric acid:acetonitrile (71.5:28.5 by volume), at a flow-rate of 1.2 mL/min, in conjunction with a Waters Nova-Pak C18 column (300 x 3.9 mm). The analytical column was used in combination with a Guard-Pak module containing a Nova-Pak C18 Guard-Pak insert. Using fluorescence detection (excitation 245 nm, emission 335 nm), plasma levels in the region of 5-10 micrograms/L for the drug and its metabolites can be detected with only 200 microL of plasma. The method has been applied to studies of the disposition of morphine and its metabolites in premature neonates requiring mechanical ventilation who were receiving the drug intravenously; preliminary findings in patients at steady state are presented.

Chromatography, High Pressure Liquid↗
PubMedDate not supplied

High performance liquid chromatographic determination of levomepromazine in human breast milk and serum using solid phase extraction.

A high performance liquid chromatographic (HPLC) method has been developed for the determination of levomepromazine in human breast milk and serum. The levomepromazine was extracted by a rapid and simple extraction method using a Sep-Pak C18 cartridge. The extracts were separated by HPLC on a C8 bonded reversed phase column and detected by UV absorbance at 254 nm. There was no interference with endogenous substance in human breast milk and serum. A linear relationship was obtained for the levomepromazine over the concentration range of 10-300 ng/mL. The recoveries of levomepromazine added to human breast milk and serum were 92.5-99.1% and 86.9-103.9%, respectively.

Chromatography, High Pressure Liquid↗
PubMed2004

Simultaneous determination of caffeine, theophylline and theobromine in human plasma by on-line solid-phase extraction coupled to reversed-phase chromatography.

A reversed-phase liquid chromatographic column switching system was described for the determination of caffeine (CF), theophylline (TH) and theobromine (TB) in human plasma with a direct injection procedure. A short protein-coated mu Bondapak CN silica pre-column (20 x 3 mm, i.d.) was used for enrichment of the drugs and clean up from weakly retained plasma components using phosphate buffer saline pH 7.4. After washing step, the retained drugs were flushed into a reversed-phase column (5 microm TSK gel ODS-80 TM, 150 x 4.6 mm i.d.) with a mobile phase of methanol-0.01 M phosphate buffer, pH 3.5 (30:70, v/v) for the final separation. The eluent was monitored with a UV detector at 275 nm. The resulting chromatograms showed no interference from endogenous plasma components. A linear relationship between the concentration of drug and peak height was confirmed in the range of 0.5-20 microg/mL for all drugs. High extraction recoveries from plasma ranging from 96.12 to 100.32% were achieved. Validation of the method was examined performing intra- and inter-day accuracy and precision and was found to be satisfactory. The coefficients of variation of the three drugs were less than 3% for intra-day and less than 4% for inter-day run assays.

Buffers↗
PubMed2005

Validation and application of a method for the determination of nicotine and five major metabolites in smokers' urine by solid-phase extraction and liquid chromatography-tandem mass spectrometry.

An SPE-LC-MS/MS method was developed, validated and applied to the determination of nicotine and five major metabolites in human urine: cotinine, trans-3'-hydroxycotinine, nicotine-N-glucuronide, cotinine-N-glucuronide and trans-3'-hydroxycotinine-O-glucuronide. A 500 microL urine sample was pH-adjusted with phosphate buffer (1.5 mL) containing nicotine-methyl-d3, cotinine-methyl-d3 and trans-3'-hydroxycotinine-methyl-d3 internal standards. For the unconjugated metabolites, an aliquot (800 microL) of the buffered solution was applied to a 30 mg Oasis HLB-SPE column, rinsed with 2% NH4OH/H2O (3.0 mL) and H2O (3.0 mL) and eluted with methanol (500 microL). The eluate was analyzed isocratically (100% methanol) by LC-MS/MS on a diol column (50 x 2.1 mm). For the total metabolites, a beta-glucuronidase/buffer preparation (100 microL) was added to the remaining buffered solution and incubated at 37 degrees C (20 h). An aliquot (800 microL) of the enzymatically treated buffered solution was extracted and analyzed in the same manner. The conjugated metabolites were determined indirectly by subtraction. The quantitation range of the method (ng/mL) was 14-10,320 for nicotine, 15-9800 for cotinine and 32-19,220 for trans-3'-hydroxycotinine. The validated method was used to observe diurnal variations from a smoker's spot urine samples, elimination half-lives from a smoker's 24 h urine samples and metabolite distribution profiles in the spot and 24 h urine samples.

Chemical Fractionation↗
PubMed2006

Rapid determination of haloperidol and its metabolites in human plasma by HPLC using monolithic silica column and solid-phase extraction.

A rapid, sensitive and reproducible HPLC method was developed and validated for the analysis of haloperidol and its three main metabolites in human plasma. The analysis was carried out on a monolithic silica column (Chromolith Performance RP-18e, 100 x 4.6 mm). The mobile phase consisted of sodium phosphate (0.1 m, pH 3.5)-acetonitrile (80:20, v/v) at a flow rate of 2.0 mL/min. UV detection at 230 nm was used, with the detection limits of these compounds ranging from 2 to 5 ng. The separation factors of all studied compounds were in the range 2.30-16.32, while the resolution factors were from 1.00 to 5.37.

Chemical Fractionation↗
PubMed2005

Capillary-based solid-phase extraction with columns prepared using different bead trapping methods.

Three approaches of bead immobilization for CEC column preparation in a capillary were examined for SPE. The three approaches included a packed column with a single frit, a packed column with an inlet and outlet frit, and an entrapped column where beads were immobilized within an organic polymer. A direct comparison of SPE/preconcentration of 4,4-difluoro-1,3,5,7,8-pentamethyl-4-bora-3a,4a-diaza-s-indacene and 4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-propionic acid with a 2 cm long bed showed that the entrapped column yielded the best performance in terms of reproducibility and robustness. The room temperature chemistry utilized to form the entrapped column enables the column to be photopatterned anywhere within the capillary without loss in bead functionality, and effectively links individual beads to one another at specific bead-bead and bead-capillary contact points. A 0.5 cm long entrapped bed exhibits high mechanical strength and is able to withstand >4400 psi. The entrapped bed was used to preconcentrate progesterone and beta-estradiol providing signal enhancements of >600. Following preconcentration, the hormones could be separated using CEC. With the current availability of numerous well-characterized chromatographic packing materials and the relative simplicity of the fabrication method, this methodology can be readily adapted to HPLC, CEC, and micro total analysis system.

Electrophoresis, Capillary↗
PubMed2006

Determination of antidepressants in surface and waste water samples by capillary electrophoresis with electrospray ionization mass spectrometric detection after preconcentration using off-line solid-phase extraction.

A method for the quantitative determination of seven major antidepressants in surface waters and sewage treatment plant effluents by CE using ESI-MS is presented. Calibration curves for the selected analytes were prepared in Milli-Q purified water and Danube river water extract covering a concentration range of at least one order of magnitude. LODs achieved were between 6 and 13 microg/L for Trazodone and 39 and 53 microg/L for Sertraline in the Milli-Q purified water and Danube river water matrix, respectively. For sample preparation eight different SPE materials were investigated. Best results were obtained for a resin based on hydrophilic divinylbenzene (recoveries from Milli-Q purified water 93-96%; from Danube river water 85-99%). Finally, a series of eight sewage treatment plant effluents were investigated with respect to their content in the selected antidepressants. Six of these samples were tested positive for antidepressants, in particular Venlafaxine, Citalopram and Trazodone in concentrations between 36 and 322 ng/L.

Antidepressive Agents↗