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At least 1,693 records · Page 94Linked to original sources
PubMed1992

Determination of gliclazide in serum by high-performance liquid chromatography using solid-phase extraction.

A simple and sensitive high-performance liquid chromatographic method for a routine assay of gliclazide in serum is described. Serum samples spiked with glibenclamide (internal standard) were applied to Bond Elut C18 cartridges. After washing with phosphate buffer (pH 7.5) and water, the cartridge was eluted with 60% methanol. The eluate was evaporated to dryness. The residue was dissolved in methanol and injected onto an octadecyl silica column (5 microns, 150 mm x 4.6 mm I.D.). The mobile phase was 0.04 M potassium dihydrogenphosphate (pH 4.6)-acetonitrile-isopropyl alcohol (5:4:1, v/v). Ultraviolet detection at 227 nm was used. The minimum detectable level of gliclazide was 20 ng/ml.

Chromatography, High Pressure Liquid↗
PubMed1993

Solid-phase extraction and gas chromatographic-mass spectrometric determination after hydrolysis of 2-aminofluorene haemoglobin adducts in blood of rats.

2-Nitrofluorene is an environmental pollutant that binds covalently to haemoglobin after nitroreduction and successive N-hydroxylation. these haemoglobin adducts can be cleaved in vitro by mild base-catalysed hydrolysis. For the enrichment of arylamines from the aqueous hydrolysate, an extraction procedure with an organic solvent is widely used. Because of the formation of a thick emulsion layer between the aqueous and organic solvent layers, the extraction is laborious and inefficient. The use of Amberlite XAD2 provides a simple extraction procedure yielding a recovery of ca. 70%. Calibration curves in haemoglobin solution were prepared with a correlation coefficient of 0.998 (n = 12). The inter-day coefficient of variation amounted to 14%.

Animals↗
PubMed1993

High-performance liquid chromatographic method for the simultaneous determination of pentisomide and its major metabolite N-desisopropylpentisomide in plasma, urine and tissues using solid-phase extraction.

A rapid, sensitive and selective high-performance liquid chromatographic method for the simultaneous determination of pentisomide and its major metabolite desisopropylpentisomide in plasma, urine and tissues has been developed. The method for plasma samples, urine samples and tissue samples, after homogenizing with 50% ethanol, involves extraction of samples via activated Bond-Elut C8 disposable columns with methanol at pH 10 after addition of internal standard, and initially on column washing of samples at pH 10 with water and acetonitrile. The obtained methanolic extract is evaporated to dryness under nitrogen at 25 degrees C; the sample residue is then reconstituted in mobile phase and an aliquot of this solution is injected into the liquid chromatograph. Separation is performed using a Nova-Pak C18 4 microns particle size column operating in combination with radial compression separation unit and a methanol-water-di-sec.-butylamine-phosphoric acid (40:60:0.5:0.2, v/v) pH 3.5 mobile phase with ultraviolet detection at 258 nm. Endogenous substances or a variety of drugs concomitantly used in pentisomide therapy, with the exception of disopyramide, do not interfere with the assay. The mean recovery of pentisomide and desisopropylpentisomide from plasma and urine and from tissues is more than 91 and 86%, respectively. The limit of detection of the assay is 10 ng/ml for both drugs. The intra- and inter-day coefficient of variation for replicate analyses of spiked plasma samples is less than 7 and 8%, respectively. Mean steady-state plasma levels of pentisomide and desisopropylpentisomide in patients on chronic oral therapy are reported.

Anti-Arrhythmia Agents↗
PubMed1993

Automated sample clean-up with solid-phase extraction for the determination of aflatoxins in urine by liquid chromatography.

An automated extraction and clean-up procedure was developed for the determination of aflatoxins in human urine at the 50 pg/ml level. Aflatoxins B1, B2, G1 and G2 are captured on C2 extraction columns and simultaneously cleaned up with the aid of a robotic system. The processed samples are analysed by reversed-phase high-performance liquid chromatography. Fluorescence detection was enhanced for aflatoxins B1 and G1 using factorial design optimization of the post-column reactor. Silylation of the glass vials used in the robotic system was of the utmost importance. With non-silylated glass vials, up to 75% of the analytes were lost. Average aflatoxin recoveries were B1 95%, B2 90%, G1 93% and G2 89%.

Aflatoxins↗
PubMed1993

Study of lot-to-lot reproducibilities of Bond Elut Certify and Clean Screen DAU mixed-mode solid-phase extraction columns in the extraction of drugs from whole blood.

The lot-to-lot reproducibilities of Bond Elut Certify and Clean Screen DAU columns are described. The recoveries of five test drugs obtained from twelve lots of Bond Elut Certify columns ranged from 84 to 104% with standard deviations of less than 9%. The recoveries of five test drugs obtained from six lots of Clean Screen DAU columns ranged from 81 to 103% with standard deviations of less than 7%. The 95% confidence intervals of the means as obtained by ANOVA demonstrate that there are no significant differences between the tested lots of Bond Elut Certify and Clean Screen DAU columns. Comparison of the two brands shows that both Bond Elut Certify and Clean Screen DAU columns are well acceptable for routine drug screening in systematic toxicological analysis, with a slightly higher overall recovery for the former.

Animals↗
PubMed1994

Column liquid chromatographic determination of bupivacaine in human serum using solid-phase extraction.

A convenient and economical procedure for the extraction of bupivacaine and its major metabolites, desbutylbupivacaine and 4'-hydroxybupivacaine, from serum is described. A 0.25-ml aliquot of 4 micrograms/ml solution of N-pentyl-2,6-pipecoloxylidide used as the internal standard and an equal volume of the serum sample are applied to a 1-ml BondElut C18 silica extraction column which has been conditioned by subsequent washing once with 1 M HCl, twice with methanol and once with water. After passing the sample at a slow rate, the column is washed twice with water and once with acetonitrile. The desired compounds are then eluted with a 0.25-ml aliquot of a mixture of 35% perchloric acid-methanol (1:40, v/v). A 5-microliters aliquot of the eluate is injected onto a 150 x 4.6 mm I.D. column packed with 5-microns C8 silica particles, which is eluted at ambient temperature with a mobile phase of acetonitrile-10 mM KH2PO4 (25:80, v/v) at a flow-rate of 1.5 ml/min. The peaks are detected at 205 nm. The extraction recovery of all the compounds is in the range of 90%. The chromatogram is clean and the desired peaks are well separated from each other and from the extraneous peaks.

Acetonitriles↗
PubMed1994

High-performance liquid chromatographic determination of the new quinolone antibacterial agent DU-6859a in human serum and urine using solid-phase extraction with photolysis-fluorescence detection.

A sensitive and specific HPLC method for the determination of DU-6859a (I), a fluoroquinolone antibacterial agent, in human serum and urine was developed. Compound I and the internal standard extracted from serum and urine by means of a Bond Elut C8 LRC cartridge showed recoveries of 96%. The extracts were chromatographed on a reversed-phase column with photolysis-fluorescence detection. This unique detection method was 42.5 times more sensitive than intrinsic fluorescence detection, the limits of detection being in 3.43 ng/ml for serum and 4.35 ng/ml for urine. In addition, I was stable in serum and urine for at least 1 month at -20 degrees C. The proposed method was sensitive and selective enough to apply to pharmacokinetic studies of I in humans after a single oral dose of 100 mg.

Anti-Infective Agents↗
PubMed1994

Column liquid chromatographic determination of paroxetine in human serum using solid-phase extraction.

A 0.5-ml aliquot of a serum sample, after the addition of a 100-microliters aliquot of a 5 micrograms/ml solution of dibucaine as the internal standard, is vortex-mixed with 0.5 ml of acetonitrile and centrifuged. The supernatant is applied to a 1-ml BondElut C18 silica extraction column conditioned with subsequent washings with 1 M HCl, methanol and water. After passing the sample at a slow rate, the column is washed twice with water and once with acetonitrile. The desired compounds are then eluted with a 0.25-ml aliquot of 35% perchloric acid-methanol (1:40, v/v). A 7-microliters aliquot of the eluate is injected onto a 150 x 4.6 mm I.D. column packed with 5-microns C8 silica particles and eluted at ambient temperature with a mobile phase of 10 mM phosphate buffer-acetonitrile (2:1, v/v) (pH 3.2). The peaks are detected with a fluorescence detector (excitation at 295 nm, emission at 365 nm). The resulting chromatogram is clean with no extraneous peaks. Paroxetine and dibucaine give sharp peaks which are well separated from each other and from the solvent peaks. The extraction recovery of the drug and the internal standard is in the range of 90% which allows a highly sensitive determination of paroxetine.

Chromatography, High Pressure Liquid↗
PubMed1995

Determination of a new fluoroquinolone antimicrobial agent, (S)-10-[(S)-(8-amino-6-azaspiro d3,4]octan-6-yl)]-9-fluoro-2, 3-dihydro-3-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]benzoxazine-6- carboxylic acid hemihydrate, DV-7751a, in human serum and urine using solid-phase extraction and high-performance liquid chromatography with fluorescence detection.

A high-performance liquid chromatographic method for the determination of a new fluoroquinolone antimicrobial agent, (S)-10-[(S)-(8-amino-6-azaspiro[3,4]octan-6-yl)]-9-fluoro-2,3- dihydro-3-methyl-7-oxo-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid hemihydrate (DV-7751a, I) in human serum and urine has been developed. Compound I and the internal standard were extracted from serum and urine by means of Bond Elut C8 LRC column. The extracts were chromatographed on a reversed-phase Inertsil ODS-2 column using tetrahydrofuran-50 mM KH2PO4 (pH2)-1 M ammonium acetate (19:81:1, v/v) as the mobile phase at a flow-rate of 1.0 ml/min. Fluorescence detection at an excitation wavelength of 305 nm and an emission wavelength of 530 nm resulted in a limit of quantitation of 0.0098 microgram/ml for serum and 0.098 microgram/ml for urine. The method showed satisfactory sensitivity, precision, accuracy, recovery and selectivity. Stability studies showed that I was stable in serum and urine for at least 1 month at -20 degrees C and for at least 48 h at room temperature.

Anti-Infective Agents↗
PubMed1995

Assay of the enantiomers of ibutilide and artilide using solid-phase extraction, derivatization, and achiral-chiral column-switching high-performance liquid chromatography.

Ibutilide fumarate and artilide fumarate, new drugs for the treatment of cardiac arrhythmias, each contain a stereogenic center bearing a secondary alcohol group. Reversed-phase achiral-chiral column-switching HPLC separations of the enantiomers of each compound were developed and validated for quantitation in plasma and other biofluids. The key component of the method was derivatization with 1-naphthyl isocyanate, which enhanced the sensitivity of fluorescence detection and enabled the enantiomers to be separated on a Pirkle column (covalent 3,5-dinitrobenzoyl-D-phenylglycine stationary phase). The lower limit of quantitation of ibutilide fumarate was typically 0.1 ng/ml or less of each enantiomer in 1 ml of plasma. Two of the special features of the column-switching system included operation with two samples in the system at one time, which reduced analysis time to 16 min/sample for ibutilide and 19 min/sample for artilide, and a relay-operated switching of detector outputs, which allowed achiral and chiral column chromatographic data to be gathered from two detectors into a single data acquisition channel.

Anti-Arrhythmia Agents↗
PubMed1995

On-line solid-phase extraction of ceftazidime in serum and determination by high-performance liquid chromatography.

A column-switching high-performance liquid chromatographic assay is described for the determination of ceftazidime (a third-generation cephalosporin) in human serum. The method does not require prior sample pretreatment. Serum is directly injected in a first chromatographic column for sample clean-up and extraction. Thereafter, using an on-line column-switching system, the drug is quantitatively transferred and separated on a second, analytical column followed by determination using ultraviolet absorption at 258 nm. The technique allows direct, rapid, precise, and simple determination of ceftazidime in serum over the range of 1-250 micrograms/ml using 12.5 microliters of serum. This method was applied to study the pharmacokinetics of the drug in patients undergoing vascular surgery.

Ceftazidime↗
PubMed1995

Column liquid chromatographic determination of clozapine and N-desmethylclozapine in human serum using solid-phase extraction.

A 0.5-ml aliquot of a serum sample, after the addition of a 50-microliters aliquot of a 5 microgram/ml solution of amoxapine as the internal standard, is vortex-mixed with 0.5 ml of acetonitrile and centrifuged. The supernatant is applied to a 1-ml BondElut C18 silica extraction column-conditioned with subsequent washings with 1 M HCL, methanol and water. After passing the sample at a slow rate, the column is washed twice with water and once with acetonitrile. The desired compounds are then eluted with a 0.25-ml aliquot of 35% perchloric acid-methanol (1:100, v/v). A 15 microliters aliquot of the eluate is injected onto a 150 x 4.6 mm I.D. column packed with 5-microns C8 silica particles and eluted at ambient temperature with a mobile phase of 0.1% tetramethylammonium perchlorate-acetonitrile (73:27, v/v) adjusted to pH 4.2 with 10% perchloric acid. The peaks are detected with an absorbance detector at 245 nm.

Antipsychotic Agents↗
PubMed1995

Determination of the angiotensin-converting enzyme inhibitor lisinopril in urine using solid-phase extraction and reversed-phase high-performance liquid chromatography.

A simple, accurate and precise high-performance liquid chromatographic method is described for assaying lisinopril in human urine. Urine (1 ml) containing lisinopril and enalaprilat (internal standard) was acidified with 10 microliters of 6 M nitric acid, passed through a Sep-Pak C18 cartridge and eluted with 3 ml of 10% acetonitrile, followed by 6 ml of distilled water. the separations were carried out using a mu Bondapak c18 column with a mobile phase comprising acetonitrile (60 ml), methanol (10 ml) and tetrahydrofuran (10 ml) in 15 mM phosphate buffer (920 ml) at pH 2.90. Separations were performed at 40 degrees C and detection was at 206 nm. Standard calibration plots of lisinopril in urine were linear (r > 0.998) and recovery was greater than 64%. The lowest quantifiable concentration was 0.5 micrograms/ml. Within-day and between-day imprecision (coefficient of variation) ranged from 2.51% to 9.26%, and inaccuracy was less than 8.3%.

Angiotensin-Converting Enzyme Inhibitors↗
PubMed1996

Sensitive fluorimetric determination of gentamicin sulfate in biological matrices using solid-phase extraction, pre-column derivatization with 9-fluorenylmethyl chloroformate and reversed-phase high-performance liquid chromatography.

A high-performance liquid chromatographic method is described for the determination of gentamicin in bacterial culture medium or plasma with increased sensitivity and improved separation of the C1 component. Gentamicin was extracted from the biological matrix with high efficiency using carboxypropyl (CBA)-bonded silica. Derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) followed by C18 reversed-phase chromatography allowed the fluorimetric detection of gentamicins C1, C1a and C2. A fourth component, considered to be gentamicin C2a, was partially resolved from the C2 peak. Optimal conditions for the extraction and derivatization of gentamicin are described. The detection limit was below 50 micrograms/l, the assay was linear to 5 mg/l and showed good reproducibility. It is concluded that pre-column derivatization with FMOC-Cl substantially improves the analysis of gentamicin compared with present methods based on reaction with o-phthaldialdehyde.

Chromatography, High Pressure Liquid↗
PubMed1996

Simple and selective assay of 4-hydroxymephenytoin in human urine using solid-phase extraction and high-performance liquid chromatography with electrochemical detection and its preliminary application to phenotyping test.

A simple and selective HPLC method for the determination of 4-hydroxymephenytoin (4-OH-M) in human urine, using a controlled potential coulometric detector equipped with a dual working electrode cell of fully porous graphite, has been developed. After acid hydrolysis of urine, 4-OH-M and the internal standard (I.S.), 5-hydroxy-1-tetralone, were extracted from urine by means of a Bond Elut Certify LRC column. The extracts were chromatographed on a reversed-phase mu Bondapak C18 column using methanol-50 mM KH2PO4 (pH 4.0) (30:70, v/v) as the mobile phase at a flow-rate of 1.0 ml/min. Electrochemical detection at applied potential of 800 mV resulted in a limit of quantitation of 0.76 micrograms/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity. The present method was applied to the phenotyping test in thirteen Japanese healthy volunteers who received an oral 100-mg racemic mephenytoin. The phenotypes determined by the present method were found to be in agreement with those obtained with the reported customary assay based on gas chromatography.

Adult↗
PubMed1996

Determination of fenbufen and its metabolites in serum by reversed-phase high-performance liquid chromatography using solid-phase extraction and on-line post-column ultraviolet irradiation and fluorescence detection.

An improved analytical method for the detection and quantification of fenbufen and its two major metabolites is described. The assay consists of reversed-phase high-performance liquid chromatography and post-column irradiation with ultraviolet light and fluorescence detection. A highly selective chromatography separation was established on a cyanopropyl column at ambient temperature with a flow-rate of 0.5 ml/min. The analytes of interest were isolated from serum using a Bond-Elut CIN column with high recovery and selectivity. The fluorescence response of all three analytes upon UV irradiation was investigated. The post-column UV irradiation was optimized and the effect of irradiation time on the fluorescence response was determined for all three analytes. The detection limits were 10 ng/ml for each analyte using 1 ml of serum. Linear calibration curves from 50 to 375 ng/ml for all three analytes show coefficients of determination of 0.99. Precision and accuracy of the method were within 3.9-6.5 and 5.1-7.4% for fenbufen, 3.5-6.4 and 4.9-6.3% for metabolite II (expressed as lactone III) and 5.4-7.4 and 2.6-7.4% for metabolite IV, respectively.

Anti-Inflammatory Agents, Non-Steroidal↗