Nalidixic Acid and Hydroxynalidixic Acid Analysis in Human Plasma and Urine by Liquid Chromatography

Shargel, Leon; Koss, Raymond F.; Crain, A.V.R.; Boyle, V.J.

doi:10.1002/jps.2600620912

Cited by 29 publications

(3 citation statements)

References 3 publications

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“…MK-366 was extracted from serum and urine at pH 7. 5 with methylene chloride and back-extracted with sodium hydroxide solution. Chromatography was performed on an anion-exchange column with acetonitrilephosphate buffer as the mobile phase; UV absorbance was monitored at 273 nm.…”

mentioning

confidence: 99%

Determination of norfloxacin, a new nalidixic acid analog, in human serum and urine by high-performance liquid chromatography

Boppana¹,

Swanson²

1982

Antimicrob Agents Chemother

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A high-performance liquid chromatographic method for the analysis of norfloxacin [1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid], a new nalidixic acid analog, in human serum and urine is described. A statistical evaluation of the assay data showed acceptable accuracy and precision for 0.1 to 10.0 ,ug of MK-366 per ml of serum and for 1.0 to 500 ,ug of MK-366 per ml of urine. MK-366 was extracted from serum and urine at pH 7.5 with methylene chloride and back-extracted with sodium hydroxide solution. Chromatography was performed on an anion-exchange column with acetonitrilephosphate buffer as the mobile phase; UV absorbance was monitored at 273 nm. The method was used to measure MK-366 in clinical specimens.boxylic acid] is a new broad-spectrum antibacterial agent that is structurally related to nalidixic acid (Fig. 1). MK-366 exhibits greater antibacterial activity against both gram-positive and gram-negative bacteria than other nalidixic acid analogs and exhibits greater activity against Pseudomonas aeruginosa than gentamicin (1,2 Extraction of samples. Serum (1 ml) or urine (200 pul) was thoroughly mixed with 100 p.l of 0.05 N NaOH (containing standards preparing the standard curve) in a 40-ml glass extraction tube. Methylene chloride (11 ml) and 0.5 M sodium phosphate buffer (0.5 ml, pH 7.5) were then added, and the tubes were gently shaken for 10 min on a mechanical shaker. After phase separation by centrifugation at 1,500 x g for 5 min, 10 ml of the methylene chloride layer was transferred to a second 40-ml extraction tube. Fresh methylene chloride (11 ml) was added to the first extraction tube, and a second extraction was performed; 10 ml of the second extract was pooled with the first organic phase.

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confidence: 99%

Determination of norfloxacin, a new nalidixic acid analog, in human serum and urine by high-performance liquid chromatography

Boppana¹,

Swanson²

1982

Antimicrob Agents Chemother

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“…21 However, the most common methodology for the determination of nalidixic acid has been chromatography. There are several HPLC methods for the determination of nalidixic acid in human plasma and urine, 22,23 human blood, 24 or human urine, 25 and a GC method for the determination of nalidixic acid in human plasma. 26 The main inconvenience of the non-chromatographic methods is their lack of selectivity, which requires the carrying out of a previous extraction process of the analyte from the matrix using organic solvents; with the chromatographic methods, the main inconvenience is their laborious nature and extensive sample handling.…”

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confidence: 99%

Single-use phosphorimetric sensor for the determination of nalidixic acid in human urine and milk

Capitán-Vallvey

Albarbarawi

Fernández-Ramos

et al. 2000

Analyst

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A single-use phosphorimetric sensor to determine the germicide nalidixic acid is proposed. The sensing action is based on the absorption of the analyte into the sensing zone and the subsequent measurement of the phosphorescence intensity emitted by the analyte fixed in the sensor. This plane drop sensor is made up of a 3 x 1.6 cm sheet of the polyester Mylar as solid support, and a circular film 5 mm in diameter and 20 microns in thickness, formed by poly(vinyl chloride) and tributyl phosphate as the plasticizer, adhered to its surface. The sensor is introduced for 2 h into the sample solution, after which it is dried and the phosphorescence intensity is measured directly at lambda ex = 332 nm, lambda em = 412 nm, with a delay time of 0.15 ms and a gate time of 10 ms, under a dry nitrogen stream. The characteristic parameters of the construction of the sensing zone and of the processes of fixing the analyte along with the emission of phosphorescence were studied. The applicable concentration range was from 60 to 1500 ng ml-1, with a detection limit of 20 ng ml-1 and a precision of 2% expressed as relative standard deviation. The method was applied to the determination of nalidixic acid in milk and human urine with recoveries ranging between 96.0 and 103.7%. The calibration process was carried out by applying a mathematical method of finite elements that expresses the analytical signal as a function of the analyte concentration and equilibration time between the sensor and the sample solution.

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“…In those cases it is necessary to determine the plasma concentration of nalidixic acid, preferably by means of a rapid, simple method. In the literature, fluorimetric [2, 31 and liquid chromatographic [4,5] methods have been described_ The fluorimetric methods have the disadvantage of not being specific and the recently described high-performance liquid chromatographic (HPLC) method involves a time consuming derivatization step.In this paper we shall describe a gas chromatographic (GC) method that is specific and sensitive enough to determine therapeutic levels in a 1 ml plasma sample within 30 min of receipt of the sample. …”

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Rapid gas chromatographic method for the determination of nalidixic acid in plasma

Roseboom

Sorel

Lingeman

et al. 1979

Journal of Chromatography B: Biomedical Sciences and Applicatio

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Nalidixic acid is mostly used for the treatment of urinary tract infections, but in some cases it is administered intravenously for the-treatment of general infections [I] . In those cases it is necessary to determine the plasma concentration of nalidixic acid, preferably by means of a rapid, simple method. In the literature, fluorimetric [2, 31 and liquid chromatographic [4,5] methods have been described_ The fluorimetric methods have the disadvantage of not being specific and the recently described high-performance liquid chromatographic (HPLC) method involves a time consuming derivatization step.In this paper we shall describe a gas chromatographic (GC) method that is specific and sensitive enough to determine therapeutic levels in a 1 ml plasma sample within 30 min of receipt of the sample. EXPERIMENTAL ApparatusA Packard-Becker i&lode1 419 gas chromatograph, equipped with flame ionisation detectors was used. The glass column (1.5 X 6 mm 0-D.) was packed with 20% OV-1'7 on Chromosorb W HP, 80-100 mesh (Chrompack, Middelburg, The Netherlands). The operating conditions were: injection port temperature, 290"; column temperature, 270"; detector temperature, 290"; carrier gas (nitrogen) flow-rate 20 ml/min; hydrogen flow-rate 30 ml/min; air flow-rate 300 ml/min.Quantitation was carried out both by means of peak height measurements and peak area measurements with the chromatography Data Analyser System IV (Spectra Physics, Santa Clara, Calif., U.S.A.).

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Nalidixic Acid and Hydroxynalidixic Acid Analysis in Human Plasma and Urine by Liquid Chromatography

Cited by 29 publications

References 3 publications

Determination of norfloxacin, a new nalidixic acid analog, in human serum and urine by high-performance liquid chromatography

Determination of norfloxacin, a new nalidixic acid analog, in human serum and urine by high-performance liquid chromatography

Single-use phosphorimetric sensor for the determination of nalidixic acid in human urine and milk

Rapid gas chromatographic method for the determination of nalidixic acid in plasma

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