M.S. García

Simultaneous determination of propacetamol and paracetamol by derivative spectrophotometry

A first-derivative spectrophotometric method for the simultaneous determination of propacetamol hydrochloride (PRO) and paracetamol (PA) is described. Measurements are made at the zero-crossing wavelengths at 242.0 for PRO and 239.0 nm for PA. The calibration graphs were linear up to 20.0 and 15.0 mg l(-1) of PRO and PA, respectively, the limits of quantification were 0.75 and 0.46 mg l(-1). The possible interfering effects of other substances were studied. The method was applied to determining the stability of PRO in ethanolic solutions and in glucose and saline parenteral solutions.

Flow-injection spectrophotometric determination of frusemide or sulphathiazole in pharmaceuticals

Two sensitive and fast flow-injection spectrophotometric methods are proposed for the determination of frusemide or sulphathiazole based on the formation of coloured complexes between these compounds and Pd(II) at pH 5.0 and 55 degrees C. Using the peak height as a quantitative parameter, frusemide or sulphathiazole was determined at 410 nm over the range 2.0 x 10(-5)-4.0 x 10(-4) M or 5.0 x 10(-5)-3 x 10(-4) M, respectively. The methods were applied to the determination of these sulphonamides in pharmaceuticals.

Flow-injection spectrofluorimetric determination of flufenamic and mefenamic acid in pharmaceuticals

Two sensitive and rapid flow-injection (FI) spectrofluorimetric methods are proposed for the determination of flufenamic acid (FF) and mefenamic acid (MF), based on the formation of complexes of these compounds with A1(III) in an ethanolic medium. The calibration graphs resulting from the measurements of the fluorescence at lambda exc = 351 nm and lambda em = 440 nm, and lambdaexc = 355 nm and lambda em = 454 nm for the complexes with FF and MF, respectively, are linear over the range 0.030-1.20 micrograms ml-1 for FF and 0.30-16.1 micrograms ml-1 for MF. The methods have been applied to the determination of these drugs in pharmaceutical preparations.

Flow-injection spectrophotometric determination of carbimazole and methimazole

Abstract A flow-injection method using spectrophotometric detection at 325 nm, is proposed for the determination of carbimazole or methimazole. The procedures are based on the formation of yellow complexes between these antithyroid drugs and Pd(II) in 0.5 M HC1. Methimazole or carbimazole are determined over the range 1 × 10 −5 −5 × 10 −4 M. The sampling frequency is 90 h −1 . The proposed methods are applied to the determination of methimazole or carbimazole in pharmaceuticals and methimazole added to human urine.

Determination of penicillamine or tiopronin in pharmaceutical preparations by flow injection analysis

Two flow injection analysis (FIA) methods, using spectrophotometric detection, are proposed for the determination of penicillamine or tiopronin [N-(2-mercaptopropionylglycine)]. The procedures are based on the formation of yellow complexes between these thiol-containing drugs and Pd(II), in a 1 M or 0.25 M HCl medium, respectively. With peak height as a quantitative parameter, penicillamine is determined over the range 1.0 x 10(-5)-7.0 x 10(-4) M; for tiopronin the range is 1.0 x 10(-5)-6.0 x 10(-4) M. The methods have been applied to the routine determination of the drugs in pharmaceutical preparations.

Determination of zinc (II) in pharmaceuticals based on a flow-through bulk optode.

A method based on flow injection (FI), was applied for the determination of Zn (II) using a flow-through bulk optode membrane that incorporates 1-(2-pyridylazo)-2-naphthol in a plasticized poly (vinyl chloride) membrane entrapped in a cellulose support. The calibration graph plotting the reflectance at 562 nm versus [Zn (II)] was linear in the range 0.16-3.27 mgl(-1) (2.5 x 10(-6)-5 x 10(-5) M) with a detection limit of 0.10 mgl(-1). The variation coefficients of the sensor response for 0.33 mgl(-1) of Zn (II) were +/-0.11% for consecutive measurements (n=10), +/-0.19% between days (n=5) and +/-0.22% between different membranes (n=6). The sensor can be readily regenerated with the same acetic/acetate carrier of pH 3.9. The FI method proposed was applied to the determination of zinc (II) in pharmaceuticals.

Spectrophotometric methods for determining meloxicam in pharmaceuticals using batch and flow-injection procedures

Two sensitive and fast spectrophotometric methods using batch and flow-injection procedures for the determination of meloxicam (MX) are proposed. The methods are based on the formation of a green complex between this drug and Fe(III) [2MX/Fe(III)] in a methanolic medium. The calibration graphs resulting from measuring the absorbance at 570 nm are linear over the ranges 2.0-200 and 5.00-250 mg l(-1) with detection limits of 0.47 and 0.72 mg l(-1), respectively. Furthermore, a flow-injection spectrophotometric method involving measurement of the absorbance of the drug at 362 nm in 0.1 M NaOH is presented. The calibration graph is linear over the range 0.5-20 mg l(-1) with a detection limit of 0.04 mg l(-1). The methods are applied to the routine analysis of MX in pharmaceuticals.

Spectrophotometric methods for the determination of cephradine or ceftazidine in human urine using batch and flow-injection procedures.

Sensitive and fast spectrophotometric methods for the determination of cephradine or ceftazidine in human urine, based on the formation of compounds between these drugs and Pd(II), are described. In the batch procedures the calibration graphs resulting from the measurement of the absorbance at 330 nm is linear over the range 5.0-60.0 micrograms. ml-1 for cephradine and 3.0-60.0 micrograms ml-1 for ceftazidine. The methods were successfully adapted to FI-systems, the peak heights being proportional to cephalosporin concentration over the range 5.0-60.0 micrograms ml-1 for cephradine and 3.0-60.0 micrograms ml-1 for ceftazidine. The sampling frequency was 60 h-1 with a sample injection of 72 microliters.

Determination of captopril in pharmaceutical samples by flow injection analysis

A flow injection spectrophotometric method for the determination of captopril involving measurement of the absorbance of the captopril complex with palladium(II) in a 0.12 M HCl medium at 400 nm is presented. The calibration graph was linear over the range 2 x 10(-5)-6 x 10(-4) M. The sampling frequency was 90 h-1 with sample injections of 70 microliters. The proposed method was applied to the determination of captopril in pharmaceutical samples.

Assay of acetylcholinesterase activity by potentiometric monitoring of acetylcholine

An acetylcholine-selective electrode based on a plasticized polymeric membrane has been developed. The electrode exhibited good selectivity for acetylcholine (ACh) over choline and some common ions, low drift, and a fast response to ACh. The response was linear over an ACh concentration range of 1×10(-6) to 1×10(-3) M with a slope of 59.1±0.1 and a detection limit of 1.5×10(-7)±1.2×10(-8) M. The electrode was used to monitor enzymatic ACh hydrolysis catalyzed by acetylcholinesterase (AChE) at different substrate and enzyme concentrations. A kinetic data analysis permitted the determination of the Michaelis-Menten constant of the enzymatic hydrolysis and AChE activity in the range of 2×10(-5) to 3.8×10(-1)U ml(-1).