Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “PERCHLORIC ACID”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,459 records · Page 81Linked to original sources
PubMed1999

Rapid determination of valaciclovir and acyclovir in human biological fluids by high-performance liquid chromatography using isocratic elution.

A rapid high-performance liquid chromatographic assay with isocratic elution is developed for the simultaneous quantification of valaciclovir (VACV) prodrug and its active converted compound, acyclovir (ACV), in biological fluids of treated patients. For serum, the samples are deproteinized with perchloric acid in presence of 1-methylguanosine as the internal standard (IS). For urine and dialysis liquid, the samples are diluted with a mobile phase containing the IS, then filtered. VACV, ACV and the IS are separated on a SymmetryShield RP-8 column with acetonitrile-ammonium phosphate buffer as the mobile phase and detected at 254 nm. The chromatographic time is about 12 min. The relative standard deviations (RSD) of VACV and ACV standards are between 0.5 and 3.5%. Most endogenous nucleosides and their metabolites, psychotropic drugs and drugs of abuse are shown not to interfere with this technique. The method has been applied to study the pharmacokinetics of VACV and ACV in serum, dialysis liquid and urine of renal failure patients on continuous ambulatory peritoneal dialysis (CAPD) under oral treatment of VACV.

Acyclovir↗
PubMed1999

Simple and rapid assay for acetaminophen and conjugated metabolites in low-volume serum samples.

The use of marker compounds for estimating drug metabolic capacity or pharmacokinetic parameters is common in the biological sciences. Often small laboratory animals are used and thus sample size is a limiting concern. In this report, we describe an assay we developed for measuring the concentration of acetaminophen and its conjugated metabolites in low-volume serum samples. Acetaminophen and metabolites were removed from 10 microl serum samples by a single-step 6% (v/v) perchloric acid deproteination using theophylline as internal standard. Samples were separated in a pH 2.2 sodium sulfate-acetonitrile mobile phase at a flow-rate of 1.5 ml/min on a 15 cm octadecylsilyl column at room temperature. Analytes were detected at a wavelength of 254 nm. The resulting chromatograms showed no interfering peaks from endogenous serum components. The concentration ranges measured were 1.56-200 microg/ml for acetaminophen and acetaminophen sulfate and 3.91-500 microg/ml for acetaminophen glucuronide. The assay was linear in the range of concentrations analyzed. The intra-day and inter-day coefficient of variation ranged from 0.4 to 8.2% and 0.2 to 12.3% for acetaminophen, 0.5 to 12.9% and 0.3 to 16.1% for acetaminophen glucuronide, and 0.4 to 8.1% and 0.2 to 14.3% for acetaminophen sulfate, respectively. Results from the experiments show that acetaminophen and its conjugated metabolites can easily and reproducibly be measured in low-volume serum samples and thus may offer an additional method to measure these compounds when the volume of biological samples may be limited.

Acetaminophen↗
PubMed1999

Determination of reduced and oxidized homocysteine and related thiols in plasma by thiol-specific pre-column derivatization and capillary electrophoresis with laser-induced fluorescence detection.

A new sensitive and rapid capillary electrophoresis (CE) assay for measuring reduced and oxidized thiols in human plasma has been developed. To prevent oxidation of the thiols, whole blood was immediately centrifuged after collection and the plasma proteins were precipitated with perchloric acid. The reduced thiols in the supernatant were derivatized quantitatively at 25 degrees C, pH 7.5 with a fluorescent reagent, fluorescein-5-maleimide (FM). The total plasma concentration of thiols, including the fraction coupled to proteins, was assayed after an initial reduction of the disulfide linkage in plasma with dithiothreitol. The separation of FM-thiols was performed in an acetonitrile/10 mM sodium phosphate-50 mM SDS buffer [25:75 (v/v); pH 7.0] using a fused-silica capillary (57 cm x 75 microm I.D.) at 45 degrees C. A 3-mW argon-ion laser (lambda(ex) 488 nm/lambda(em) 520 nm) was employed for FM-thiol detection. With the electric field of 530 V/cm, the time needed for the separation of FM-homocysteine, FM-glutathione and FM-N-acetylcysteine was less than 8 min. The lower limit of detection was 3 microM for the total thiols and 10 nM for the reduced thiols. The method was applied to, the determination of homocysteine levels in plasma from patients with end-stage renal disease.

Acetylcysteine↗
PubMed2000

Rapid, simple and sensitive high-performance liquid chromatographic method for detection and determination of acyclovir in human plasma and its use in bioavailability studies.

A rapid, simple and sensitive reversed-phase high-performance liquid chromatographic (HPLC) method has been developed for the measurement of acyclovir concentrations in human plasma and its use in bioavailability studies is evaluated. Unchanged acyclovir has been quantified without the introduction of an internal standard using the present method. Human plasma proteins were selectively precipitated by the addition of 7% perchloric acid to spiked plasma samples or to the plasma samples obtained after acyclovir administration to human volunteers and the mixture was spun at 1000 g for 10 min. The supernatant was directly injected into a Novaflex C18 column and detected at 254 nm. The mobile phase consisted of octane sulfonic acid buffer (pH 2.5) and methanol (92:08). The limit of quantitation for acyclovir in plasma was 20 ng/ml, which enabled the determination of the area under the curve (AUC) more precisely, that is, it is much closer to its extrapolated value. The present method has been successfully applied to samples from bioavailability studies.

Acyclovir↗
PubMed2002

Identification and determination of GnRH antagonist gelling at injection site.

The purpose of this study was to first observe whether orntide, a GnRH antagonist, gels at the injection site and if so, to develop and validate an extraction method to quantitate the peptide amount as well as assess chemical stability in the gel. After subcutaneous injection of a large dose of orntide acetate solution, a white gel and local traumatized effect were observed at the injection site. Orntide remaining at the injection site was recovered by tissue excision, homogenization and tissue protein precipitation with perchloric acid and quantified by high performance liquid chromatography (HPLC) following separation on a C18 column. The standard curve was linear in the detection range and there was no interference from either blank tissue or excipients of the orntide formulation. The recovery from spiked tissue or that immediately following injection was in the range of 90-110%. MALDI-FT mass spectrometry (MS) of the peak fraction indicated that the orntide recovered from the injection site was in the intact form. The results showed that orntide solution, when injected at a large dose, formed a gel at the injection site. The gel delayed the release from the injection site and caused discernible tissue reaction.

Animals↗
PubMed2003

Skeletal muscle metabolism in Duchenne muscular dystrophy (DMD): an in-vitro proton NMR spectroscopy study.

The metabolic differences in the skeletal muscle of patients with Duchenne muscular dystrophy (DMD) and normal subjects (controls) were investigated using in-vitro high-resolution proton NMR spectroscopy. In all, 56 metabolites were unambiguously identified in the perchloric acid extract of muscle tissue using one- and two-dimensional NMR. The concentrations of glycolytic substrate glucose (Glc; p < 0.05), gluconeogenic amino acids such as glutamine (Gln; p < 0.05) and alanine (Ala; p < 0.05) and the glycolytic product lactate (Lac; p < 0.05) were statistically significantly lower in DMD patients as compared to controls. A significant reduction in the concentrations of total creatine (TCr; p < 0.05), glycerophosphoryl choline + phosphoryl choline + carnitine (GPC/PC/Car; p < 0.05), choline (Cho; p < 0.05) and acetate (Ace; p < 0.05) was also observed in these patients. Decrease in the level of glucose may be attributed to the reduction in the concentrations of gluconeogenic substrates or membrane abnormalities in degenerated muscle of DMD patients. Lower levels of choline containing compounds indicate membrane abnormalities. Decrease in the concentration of lactate in the muscle of DMD patients may be due to the reduction in anaerobic glycolytic activity or lower substrate concentration. The decrease in the concentration of acetate may reflect reduced transport of fatty acids into mitochondria due to decreased concentration of carnitine in DMD patients. Kreb's cycle intermediate alpha-ketoglutarate was observed only in the diseased muscle, which is suggestive of predominant oxidative metabolism for energy generation.

Adolescent↗
PubMed2001

Spectrophotometric, septrofluorimetric and LC determination of lisinopril.

Three methods are described for the determination of lisinopril in the pharmaceutical tablets. The spectrophotometric method depends on the reaction of the lisinopril with sodium hypochlorite and phenyl hydrazine to form a condensation product measured at 362 nm. The spectrophotometric method was extended to develop a stability indicating method. The spectrofluorimetric method depends on reaction of the lisinopril with o-phthalaldehyde in the presence of 2-mercaptoethanol in borate buffer pH 9.5. The fluorescence of the reaction product was measured upon excitation at a maximum of 340 nm with emission wavelength at 455 nm. The HPLC method depends on using Hypersil silica column with a mobile phase consisting of methanol-water-triethylamine (50:50:0.1 v/v) and the pH was adjusted to 2.6 with 0.1 N perchloric acid. Quantitation was achieved with UV detection at 210 nm based on peak area.

Angiotensin-Converting Enzyme Inhibitors↗
PubMed2002

Spectrophotometric determination of alendronate in pharmaceutical formulations via complex formation with Fe(III) ions.

The formation of the complex between alendronate, non-chromophoric bisphosphonate drug important for the treatment of a variety of bone diseases, and iron(III) chloride in perchloric acid solution was studied. The stoichiometric ratio of alendronate to Fe(III) ions in the chromophoric complex was determined to be 1:1. The conditional stability constant was logK'(ave)=4.50(SD=0.15), indicating that the Fe(III)-alendronate complex is a complex of medium stability. The optimum conditions for this reaction were ascertained and a spectrophotometric method was developed for the determination of alendronate in the concentration range 8.1-162.5 microg ml(-1), the detection limit being 2 microg ml(-1). The method was validated for the direct determination of alendronate in tablet dosage formulations.

Alendronate↗
PubMed2002

LC determination and pharmacokinetics of meloxicam.

A simple and rapid HPLC assay method for the estimation of meloxicam in plasma was developed. The method totally eliminated the solvent extraction procedure. The plasma proteins were precipitated using perchloric acid (70%) and acetonitrile mixture (1:1 v/v) and the supernatant was directly injected to the HPLC system. The separation was achieved on a Lichrospher C18 5 micron (125x4.0 mm) analytical column with a mobile phase of sodium acetate buffer (pH 3.3, 170 mmol):acetonitrile (62:38 v/v) mixture. Detection was by UV detector at 355 nm. The retention time observed for meloxicam and piroxicam (internal standard) were at 6.0 and 4.0 min, respectively. The response was linear over a range of 50-1500 ng x ml(-1) in human plasma. The method was simple, specific, precise and accurate. The method was also used for the bioequivalence study of meloxicam formulation in healthy, human, Indian, male volunteers.

Adult↗
PubMed2003

Stereoselective determination of pyridoglutethimide enantiomers in serum with a chiral cellulose-based high-performance liquid chromatographic column using solid phase extraction and UV detection.

A sensitive method for the separation and determination of R(+)- and S(-) enantiomers of pyridoglutehimide in serum by high performance liquid chromatography (HPLC) with UV detection was developed. The assay involves the use of a solid-phase extraction for serum sample clean-up prior to HPLC analysis using a C18 Bond-Elute column. Chromatographic resolution of the enantiomers was performed on a reversed-phase cellulose-based chiral column (Chiralcel OD-R, 250 x 4.6 mm I.D.) under isocratic conditions using a mobile phase of 25:75 v/v acetonitrile-0.3 M aqueous sodium perchlorate (pH 6.2 adjusted with perchloric acid) at a flow rate of 0.8 ml/min. Recoveries for R(+)- and S(-)-pyridoglutethimide enantiomers were in the range 86-91% at 300-900 ng/ml level. Intra-day and inter-day precision calculated as %R.S.D. were in the ranges of 2.9-3.9 and 1.5-4.7% for both enantiomers, respectively. Intra-day and inter-day accuracies calculated as percentage error were in the ranges of 1.9-3.3 and 1.5-3.9% for both enantiomers, respectively. Linear calibration curves in the concentration ranges of 100-1500 ng/ml for each enantiomer show correlation coefficient (r) of more than 0.9995. The limit of quantification (LOQ) of each enantiomer was 100 ng/ml using 1 ml of serum. The detection limit (LOD) for each enantiomer in serum using a UV detection set at 257 nm was 50 ng/ml (S/N = 2).

Aminoglutethimide↗
PubMed2003

An LC-MS-MS method for the determination of nevirapine, a non-nucleoside reverse transcriptase inhibitor, in human plasma.

A sensitive and rapid liquid chromatography tandem mass spectrometry (LC-MS-MS) method has been developed to measure the levels of the HIV-1 non-nucleoside reverse transcriptase inhibitor nevirapine (NVP) in human plasma. The analyte and internal standard (IS) are isolated from plasma by a simple perchloric acid precipitation of plasma proteins followed by centrifugation. LC-MS-MS in positive mode used pairs of ions at m/z of 267/226 for NVP and 628/421 for the IS, respectively. Two linear calibration curves were established for quantitation of NVP with the low curve ranging from 25 to 1000 ng/ml and the high curve ranging from 1000 to 10,000 ng/ml. Mean inter- and intra-assay coefficients of variation (CVs) over the ranges of the two standard curves were less than 10%. The overall recovery of NVP was 92.4%.

Anti-HIV Agents↗
PubMed2003

Simultaneous high-throughput determination of clenbuterol, ambroxol and bromhexine in pharmaceutical formulations by HPLC with potentiometric detection.

Potentiometric detection of clenbuterol, ambroxol and bromhexine in marketed pharmaceuticals was described in six isocratic HPLC systems. The podant- and macrocyclic-type neutral ionophores, N,N,N',N'-tetracyclohexyl-oxybis(o-phenyleneoxy)diacetamide (TOPA) and hexakis(2,3,6-tri-O-octyl)-alpha-cyclodextrin (OCD), were applied in poly(vinyl)chloride (PVC)-based liquid membrane electrodes. Both types of neutral ionophores improve the sensitivity for all mentioned drugs when compared with a tetrakis(p-chlorophenyl)borate (BOR)-based electrode as well as with single wavelength UV detection. Detection limits (S/N=3) of 2.6 x 10(-10) mol l(-1) (injected concentration) for the highly hydrophobic bromhexine were achieved with the TOPA-based electrode and a cyano reversed-phase (RP)-HPLC with Uptisphere UP5CN-25QS silica column (250 x 4.6 mm i.d.) eluted with acetonitrile (AcN)-ethanol-perchloric acid (1.66 mM) (60:2:38, v/v/v) (pH* 2.45). Comparable result was obtained with OCD-based electrodes and an XTerra RP18 hybrid silica-polymer column eluted with AcN-phosphoric acid (20 mM) (25:75, v/v) (pH* 2.60). In the mobile phases containing 60-75% v/v AcN or methanol, stable and reproducible response of both types of neutral ionophore-based electrodes was observed for at least 3 days. The results of the validated procedure for reliable simultaneous determination of the drugs in fortified representative samples of pharmaceuticals were also presented.

Ambroxol↗
PubMed2003

Development of a simple HPLC method for separation of doxycycline and its degradation products.

A simple HPLC method for the separation of doxycycline and its degradation products 6-epidoxycycline and metacycline was developed. Numerous HPLC conditions were tested for the qualitative determination of doxycycline and its degradation products. The best result was achieved by using Phenomenex Luna 5 microm C(8) 250 x 4.6 mm column with a Phenomenex(R) C(8) 4 x 10 mm I.D. guard column, and a mobile phase consisting of acetonitrile:water:perchloric acid (HClO(4)) (26:74:0.25) adjusted to pH 2.5 with 5 M sodium hydroxide, a flow-rate of 1.0 ml/min and ultraviolet detection at 350 nm. Correlation coefficients for calibration curves within the detection range of 3-60 microl/ml were 0.9990 for doxycycline and 1.000 and 0.9994 for 6-epidoxycycline and metacycline, respectively (within the range 0.5-7 microl/ml). The resolution between metacycline and 6-epidoxycycline was 1.2 and between 6-epidoxycycline and doxycycline it was 1.9 which fulfils European Pharmacopoeia requirements. The within- and between-day precision was determined for both retention time and peak area. Preliminary results indicate that this method can also be applied for separating other tetracyclines such as minocycline, chlortetracycline, tetracycline and demeclocycline.

Chromatography, High Pressure Liquid↗
PubMed1997

Flow injection analysis with amperometric detection of naltrexone in pharmaceuticals.

Flow injection analysis (FIA) with amperometric detection using a carbon paste electrode is applied to the determination of naltrexone. The sample solution was injected into the carrier stream of 0.1 M perchloric acid, being determined by oxidation at +1.0 V vs. Ag/AgCl/sat. KCl using a flow rate of 4 ml min-1. A relative standard deviation of 1.5% was calculated for a concentration level of 10(-5) M (n = 17) without carrying out a carbon paste electrode pretreatment. Calibration curves were found to be linear between 2 x 10(-8) and 10(-5) M (almost three orders of magnitude) and the method has a detection limit of 2 x 10(-8) M. A simple and reproducible procedure is proposed for the determination of naltrexone in pharmaceuticals. The results compared favourably with those obtained by an HPLC-UV method.

Chemistry, Pharmaceutical↗
PubMed1998

Simplified reversed-phase HPLC method with spectrophotometric detection for the assay of verapamil in rat plasma.

A high-performance liquid chromatographic (HPLC) method was developed for the assay of verapamil in rat plasma. After deproteinization of the plasma sample with an acetonitrile-perchloric acid (8:2) mixture containing dextromethorphan, the internal standard, an aliquot of the supernatant was directly analyzed on a cyanopropylsilane column with methanol-acetonitrile-triethylamine acetate buffer (10:30:60) as the mobile phase and detection at 235 mm. At a flow rate of 1.5 ml min-1, a complete analysis was completed in less than 6 min. The method was linear for verapamil concentrations in the range 0.5-10 micrograms ml-1 (r = 0.9999). Recoveries for the same drug concentrations from spiked rat plasma ranged from 85.6-93.0% (n = 8). The mean RSD values for intraday and interday assay reproducibility (n = 3) were, in both cases, less than 0.9%. The limit of detectability was about 0.1 microgram ml-1. The method was found useful to monitor the plasma levels of verapamil in rats that had received this drug by the nasal, oral and intravenous routes of administration.

Animals↗
PubMed1998

Determination of total cysteamine in human serum by a high-performance liquid chromatography with fluorescence detection.

A convenient, reliable and rapid method for determination of total cysteamine in human plasma by high-performance liquid chromatography with fluorescence detection is reported. This assay involves reduction of samples with dithiothreitol, derivatization of total cysteamine by addition of monobromobimane and protein precipitation by perchloric acid. The calibration curve was linear in the range 2-150 nmol ml-1 and the detection limit was 0.5 nmol ml-1. This method was successfully applied for a pharmacokinetic study of three cysteamine derivatives in healthy volunteers without any interference from coexisting substances.

Biological Availability↗
PubMed1999

Determination of the oral platelet aggregation inhibitor Sibrafiban in rat, dog, and human plasma utilising HPLC-column switching combined with turbo ion spray single quadrupole mass spectrometry.

A sensitive and selective HPLC-column switching method with single quadrupole mass spectrometric detection was developed for the simultaneous determination of the oral platelet aggregation inhibitor Sibrafiban (double protected prodrug), its prodrug and the active metabolite in rat, dog, and human plasma. The three analytes together with their tri-deuterated internal standards were isolated from plasma by protein precipitation (0.5 M perchloric acid). The de-proteinated samples were injected onto a standard-bore trapping column (4.0 mm i.d., LC-ABZ) of an HPLC-column switching system. Polar plasma components were removed by flushing the trapping column with ammonium formate (pH 3.6; 5 mM). Enriched compounds (including the analytes of interest) were backflushed onto a narrow-bore analytical column (2.1 mm i.d., Inertsil ODS-2) and separated by gradient elution (formic acid/ methanol). The whole effluent (200 microl/min) from the analytical column was passed to the turbo ion spray interface without splitting. Selected ion monitoring (SIM) was used for mass spectrometric detection. The limit of quantification for all three analytes was 1 ng/ml, using a 250-microl specimen of plasma. The mean precision and inaccuracy for the three analytes in all species were < 6 and < 5%, respectively. The practicability of the new analytical method was demonstrated by the analysis of about 500 rat and dog plasma and about 14,000 human plasma samples. The new method represents a successful example for the application of LC single MS with ionspray ionisation to the analysis of small molecule drugs in biological matrices from toxicokinetic studies and large clinical trials.

Administration, Oral↗
PubMedDate not supplied

Determination of acetaldehyde in blood by solid phase extraction and high performance liquid chromatography.

A simple method has been developed for the measurement of acetaldehyde in blood. Samples were treated with perchloric acid to precipitate proteins. After centrifugation, the supernatant, together with the internal standard (crotonaldehyde), were reacted with 2,4-dinitrophenylhydrazine reagent. The derivatized acetaldehyde was then isolated by solid phase extraction and followed by high performance liquid chromatography quantitation. This method had a minimal detectable concentration of 0.28 microM, and displayed an intra-assay precision of 2.23% and an inter-assay precision of 5.18%. The recoveries of acetaldehyde at added concentrations of 1.42 and 7.14 microM were 106.7% and 101.9%, respectively.

Acetaldehyde↗