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Journal of Chromatography Feb 1991A simple and rapid high-performance liquid chromatographic (HPLC) method for the simultaneous determination of sulphamonomethoxine (SMMX), sulphadimethoxine (SDMX),...
A simple and rapid high-performance liquid chromatographic (HPLC) method for the simultaneous determination of sulphamonomethoxine (SMMX), sulphadimethoxine (SDMX), sulphisozole (SIZ), nalidixic acid (NA), oxolinic acid (OXA), piromidic acid (PMA), furazolidone (FZ) and sodium nifurstyrenate (NFSA) in cultured fish was developed. The drugs were extracted with 0.2% metaphosphoric acid-methanol (6:4), followed by a Bond Elut C18 clean-up procedure. The HPLC separation was carried out on an Inertsil ODS column (150 x 4.6 mm I.D.) using 5 mM aqueous oxalic acid-acetonitrile (55:45) as the mobile phase with detection at 265 nm (0.04 a.u.f.s.). The calibration graphs were rectilinear from 1 to 20 ng for OXA, from 2 to 50 ng for SMMX, SDMX, SIZ, NA, PMA and FZ and from 5 to 100 ng for NFSA. The recoveries of each drug added to fish were 65.0-89.5%. The detection limits were 0.02 micrograms/g for OXA, 0.05 micrograms/g for SMMX, SDMX, SIZ, NA, PMA and FZ and 0.1 micrograms/g for NFSA.
Topics: Anti-Infective Agents; Chromatography, High Pressure Liquid; Fish Products; Food Contamination; Hydrogen-Ion Concentration; Spectrophotometry, Ultraviolet
PubMed: 2016391
DOI: 10.1016/s0021-9673(01)88874-9 -
Journal of Chromatography Feb 1987
Topics: Animals; Chromatography, High Pressure Liquid; Culture Techniques; Fishes; Nalidixic Acid; Nicotinic Acids; Oxolinic Acid; Piromidic Acid; Spectrophotometry, Ultraviolet
PubMed: 3558658
DOI: 10.1016/s0021-9673(01)94507-8 -
Ugeskrift For Laeger Sep 1981
Clinical Trial Randomized Controlled Trial
[Patients with symptoms of acute urinary infections treated with piromidic acid or sulfamethizole in general practice. A double-blind clinical controlled multicentre study].
Topics: Acute Disease; Adolescent; Adult; Aged; Clinical Trials as Topic; Double-Blind Method; Female; Humans; Male; Middle Aged; Nicotinic Acids; Piromidic Acid; Sulfamethizole; Sulfathiazoles; Urinary Tract Infections
PubMed: 7029845
DOI: No ID Found -
Rapid Communications in Mass... Dec 2012Veterinary drug residue analysis of meat and seafood products is an important part of national regulatory agency food safety programs to ensure that consumers are not...
RATIONALE
Veterinary drug residue analysis of meat and seafood products is an important part of national regulatory agency food safety programs to ensure that consumers are not exposed to potentially dangerous substances. Complex tissue matrices often require lengthy extraction and analysis procedures to identify improper animal drug treatment. Direct and rapid analysis mass spectrometry techniques have the potential to increase regulatory sample analysis speed by eliminating liquid chromatographic separation.
METHODS
Flumequine, oxolinic acid, and nalidixic acid were extracted from catfish, shrimp, and salmon using acidified acetonitrile. Extracts were concentrated, dried onto metal sample wells, then rapidly desorbed (6 s) with an infrared diode laser for analysis by laser diode thermal desorption atmospheric pressure chemical ionization with tandem mass spectrometry (LDTD-MS/MS). Analysis was conducted in selected reaction monitoring mode using piromidic acid as internal standard.
RESULTS
Six-point calibration curves for each compound in extracted matrix were linear with r(2) correlation greater than 0.99. The method was validated by analyzing 23 negative samples and 116 fortified samples at concentrations of 10, 20, 50, 100, and 600 ng/g. Average recoveries of fortified samples were greater than 77% with method detection levels ranging from 2 to 7 /g. Three product ion transitions were acquired per analyte to identify each residue.
CONCLUSIONS
A rapid method for quinolone analysis in fish muscle was developed using LDTD-MS/MS. The total analysis time was less than 30 s per sample; quinolone residues were detected below 10 ng/g and in most cases residue identity was confirmed. This represents the first application of LDTD to tissue extract analysis. Published 2012. This article is a US Government work and is in the public domain in the USA.
Topics: Animals; Anti-Bacterial Agents; Aquaculture; Calibration; Catfishes; Drug Residues; Limit of Detection; Mass Spectrometry; Quinolones; Reproducibility of Results; Seafood; Veterinary Drugs
PubMed: 23136016
DOI: 10.1002/rcm.6414 -
Presse Medicale (Paris, France : 1983) May 1983
Topics: Acute Kidney Injury; Aged; Female; Humans; Male; Middle Aged; Nicotinic Acids; Piromidic Acid
PubMed: 6222321
DOI: No ID Found -
Journal of Chromatography. B,... May 2002A simple and rapid capillary zone electrophoresis determination method with UV detection of grepafloxacin and clinafloxacin has been developed. The separation was...
A simple and rapid capillary zone electrophoresis determination method with UV detection of grepafloxacin and clinafloxacin has been developed. The separation was performed in 35 mM borate-35 mM phosphate buffer solution (pH 8.6), containing 6% (v/v) of acetonitrile. Analyses were realised using fused-silica capillaries (57 cm length x 75 microm I.D.) and the operating conditions were: 15 kV applied voltage, 30 degrees C and detection at 279 nm. Piromidic acid was used as an internal standard. The linear concentration range of application was 1.0-120.0 microg ml(-1) for both compounds, with a detection limit of 0.2 microg ml(-1) for grepafloxacin and 0.3 microg ml(-1) for clinafloxacin. The analysis yielded good reproducibility (RSD between 3.37 and 1.74%). It was applied to the determination of grepafloxacin and clinafloxacin in human and rat urine samples. The method was validated using HPLC as a reference method. Recovery levels were between 94.5 and 103%.
Topics: Animals; Anti-Infective Agents; Calibration; Electrophoresis, Capillary; Fluoroquinolones; Humans; Piperazines; Rats; Reference Standards; Reproducibility of Results
PubMed: 12016016
DOI: 10.1016/s1570-0232(02)00050-8 -
Journal of Separation Science Jun 2007A simple chromatographic method is described for assaying 15 quinolones and fluoroquinolones (pipemidic acid, marbofloxacin, enoxacin, ofloxacin, norfloxacin,... (Comparative Study)
Comparative Study
A simple chromatographic method is described for assaying 15 quinolones and fluoroquinolones (pipemidic acid, marbofloxacin, enoxacin, ofloxacin, norfloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine and piromidic acid), in urine and pharmaceutical samples. The determination was achieved by LC using an RP C18 analytical column. A mobile phase composed of mixtures of methanol-ACN-10 mM citrate buffer at pH 3.5 and 10 mM citrate buffer at pH 4.5, delivered under an optimum gradient program, at a flow rate of 1.5 mL/min, allows to accomplish the chromatographic separation in 26 min. For detection, diode-array UV-Vis at 280 nm and fluorescence detection set at excitation wavelength/emission wavelength: 280/450, 280/ 495, 280/405 and 320/360 nm were used. Detection and quantification limits were between 0.3-18 and 0.8-61 ng/mL, respectively. The method was validated in terms of interday (n = 6) and intraday (n = 6) precision and accuracy. The procedure was successfully applied to the analysis of human and veterinary pharmaceuticals. Also, ofloxacin was determined in human urine samples belonging to a patient undergoing treatment with this active principle, among others.
Topics: Animals; Chromatography, High Pressure Liquid; Humans; Ofloxacin; Pharmaceutical Preparations; Quinolones
PubMed: 17623463
DOI: 10.1002/jssc.200600536 -
Antimicrobial Agents and Chemotherapy Aug 2003The in vitro activities of 25 quinolones and fluoroquinolones against erythrocytic stages of Plasmodium falciparum and against liver stages of Plasmodium yoelii yoelii... (Comparative Study)
Comparative Study
The in vitro activities of 25 quinolones and fluoroquinolones against erythrocytic stages of Plasmodium falciparum and against liver stages of Plasmodium yoelii yoelii and P. falciparum were studied. All compounds were inhibitory for chloroquine-sensitive and chloroquine-resistant P. falciparum grown in red blood cells. This inhibitory effect increased with prolonged incubation and according to the logarithm of the drug concentration. Grepafloxacin, trovafloxacin, and ciprofloxacin were the most effective drugs, with 50% inhibitory concentrations of <10 micro g/ml against both strains. Only grepafloxacin, piromidic acid, and trovafloxacin had an inhibitory effect against hepatic stages of P. falciparum and P. yoelii yoelii; this effect combined reductions of the numbers and the sizes of schizonts in treated cultures. Thus, quinolones have a potential for treatment or prevention of malaria through their unique antiparasitic effect against erythrocytic and hepatic stages of Plasmodium.
Topics: 4-Quinolones; Animals; Anti-Infective Agents; Cells, Cultured; Erythrocytes; Fluoroquinolones; Liver; Mice; Plasmodium; Plasmodium falciparum; Plasmodium yoelii
PubMed: 12878530
DOI: 10.1128/AAC.47.8.2636-2639.2003 -
Chemotherapy 1978The combination effects of chlorpromazine (CPZ) and periphenazine (PPZ) with beta-lactam antibiotics (ampicillin, carbenicillin, cefazolin) and nalidixic acid group...
Synergistic effects of chlorpromazine and perphenazine on several chemotherapeutic agents. I. General profile of the effects measured by the filter paper strip-agar diffusion method with Escherichia coli and Pseudomonas aeruginosa.
The combination effects of chlorpromazine (CPZ) and periphenazine (PPZ) with beta-lactam antibiotics (ampicillin, carbenicillin, cefazolin) and nalidixic acid group compounds (nalidixic acid, piromidic acid and pipemidic acid) have been estimated to be synergistic by the filter paper strip-agar diffusion method (Dye's method) with Escherichia coli and Pseudomonas aeruginosa as test organisms. The observed synergism might be associated with their inhibition of various enzymes including ATPase and DNAase as well as with their specific binding to DNA. Similar synergistic effects of CPZ and PPZ have been shown by the broth dilution method. Based on these findings, it seems to be a fascinating project to devise a new phenothiazine drug without influence in mental disease that will have a greater measure of synergistic effect when combined with the above-studied antibacterial agents.
Topics: Adenosine Triphosphatases; Ampicillin; Anti-Bacterial Agents; Carbenicillin; Cefazolin; Chlorpromazine; DNA, Bacterial; Deoxyribonucleases; Drug Synergism; Escherichia coli; Immunodiffusion; Methods; Nalidixic Acid; Perphenazine; Pseudomonas aeruginosa
PubMed: 145936
DOI: 10.1159/000237764 -
Journal of Medicinal Chemistry Jan 1975The preparation and antibacterial activity of a series of the title compounds (21-73) are described. These compounds were prepared from the 2-methylthio derivatives 2...
The preparation and antibacterial activity of a series of the title compounds (21-73) are described. These compounds were prepared from the 2-methylthio derivatives 2 and 3 via the 2-methylthio-8-substituted compounds 4-20; compounds 4-20 easily underwent displacement reactions with a variety of piperazines to afford 2-(4-substituted or unsubstituted 1-piperazinyl) derivatives 21-56, of which 21, 22, 27 and 51 with unsubstituted piperazinyl group at position 2 are converted subsequently into 57-73 by alkylation, acylation, sulfonylation, or addition of isocyanates to the piperazine nitrogen. The hexahydro-1H-1,4-diazepinyl analog 74 was also prepared. The most active members in this series of compounds were found to be 8-ethyl- and 8-vinyl-5,8-dihydro-5-oxo-2-(1-piperazinyl)pyrido(2,3-d)pyrimidine-6-carboxylic acids (22 and 51), both of which are more active in vitro and in vivo against gram-negative bacteria, including Pseudomonas aeruginosa, than piromidic acid (1). Structure-activity relationships are discussed.
Topics: Animals; Anti-Bacterial Agents; Carboxylic Acids; Escherichia coli; Male; Mice; Microbial Sensitivity Tests; Pseudomonas Infections; Pseudomonas aeruginosa; Pyridones; Pyrimidines; Salmonella Infections, Animal; Salmonella typhimurium; Staphylococcus; Structure-Activity Relationship
PubMed: 803246
DOI: 10.1021/jm00235a017