scholarly journals Fast determination of minoxidil by photometric flow titration

2005 ◽  
Vol 30 (3) ◽  
pp. 79-84 ◽  
Author(s):  
R. A. de Sousa ◽  
F. S. Semaan ◽  
J. A. F. Baio ◽  
E. T. G. Cavalheiro

A photometric flow titration based on the redox reaction between KMnO4 and minoxidil is described. The best titration results were observed at 3.20 x 10-4 mol L-1 KMnO4 and 1.00 x 10-3 mol L-1 minoxidil, using the minoxidil solutions as titrant. The flow rate was fixed at 17 mL min-1 and the titrant was added to the system in aliquots of 500 µL, the color changes were monitored at 550 nm. The method was applied to commercial samples and compared with the results from a chromatographic procedure. Recoveries from 97.6 to 102.8 % were observed depending on the sample. Comparison with the chromatographic procedure reveled relative errors of 3.5 - 4.0 %.

2018 ◽  
Vol 34 (2) ◽  
pp. 23
Author(s):  
Rogério Adelino De Sousa ◽  
Éder Tadeu Gomes Cavalheiro

A potentiometric titration method for the determination of minoxidil based on its redox reaction with K2Cr2O7 is described. The best results were observed using 1.00 x 10-3 mol L-1 K2Cr2O7 and 1.00 x 10-2 mol L-1 minoxidil solutions, and the minoxidil as titrant in 2.00 mol L-1 H2SO4 medium. The method was applied to commercial samples and compared with the results from a chromatographic procedure. Recoveries from 97.4 to 98.7 % were observed depending on the sample. Comparison with the chromatographic procedure reveled agreement within 90% confidence level.


Sensors ◽  
2020 ◽  
Vol 20 (15) ◽  
pp. 4318 ◽  
Author(s):  
Mieczysław Bakuła

This paper presents a precise and fast method of ambiguity resolution (PREFMAR) for frequencies L1/E1 and L5/E5a of GPS/GALILEO data. The developed method is designed for precise and fast determination of ambiguities in GNSS phase observations. Ambiguities are chosen based on mathematical search functions. The fact that no variance–covariance matrix (VC matrix) with a so-called float solution is needed proves the innovativeness of the developed method. The developed method enables determination of the ambiguities for short baseline double-difference (DD) observations. The presented algorithms for the developed method enable unique and reliable calculation of the ambiguity if the actual errors of code measurements of DD observations are less than 0.38 m and the relative errors of phase observations are in the range of ±3 cm. The paper presents both mathematical derivations of the functions used in the PREFMAR and numerical calculations based on real double-difference GPS observations (L1-L5). The elaborated algorithms can be easily implemented into GNSS receivers or mobile phones. Therefore, they can be widely used in many geoscience applications, as well as in precise GPS/GALILEO navigation.


2009 ◽  
Vol 34 (2) ◽  
pp. 23-27 ◽  
Author(s):  
Rogério Adelino de Sousa ◽  
Éder Tadeu Gomes Cavalheiro

A potentiometric titration method for the determination of minoxidil based on its redox reaction with K2Cr2O7 is described. The best results were observed using 1.00 x 10-3 mol L-1 K2Cr2O7 and 1.00 x 10-2 mol L-1 minoxidil solutions, and the minoxidil as titrant in 2.00 mol L-1 H2SO4 medium. The method was applied to commercial samples and compared with the results from a chromatographic procedure. Recoveries from 97.4 to 98.7 % were observed depending on the sample. Comparison with the chromatographic procedure reveled agreement within 90% confidence level.


Author(s):  
Sercan Yıldırım ◽  
Gökhan Demirdaş ◽  
Mert Fidan ◽  
Ahmet Yaşar

Background: Terbinafine is an allylamine antifungal which is effective against many fungi, dermatophytes and moulds. Analytical methods are required for the determination of terbinafine in biological fluids to perform therapeutic drug monitoring and pharmacokinetic studies. Objective: The aim of this study was to develop and validate a novel and fast method combining dilute and shoot approach and high-performance liquid chromatography coupled with photodiode array detection for the determination of terbinafine in human urine. Methods: Chromatographic parameters including mobile phase composition, pH, flow rate and injection volume was assessed and optimized. The separation of terbinafine and naproxen (internal standard) was achieved within 3 min using a C18 core-shell column (Raptor ARC-18, 100 x 4.6 mm, 2.7 µm) under isocratic conditions. Samples were eluted from the column at the flow rate of 1.4 mL/min using a mobile phase containing 0.2% triethylamine in water (pH 3.4 with formic acid): acetonitrile (45:55, v/v). Results: Presented technique was linear in the range of 25-2000 ng/mL. Intra- and inter-day reproducibility at four quality control levels (25, 200, 750 and 1500 ng/mL) was less than 7%, with relative errors ranging from -5.40% to 5.91%. Limit of detection was 12.60 ng/mL. Developed method has three main advantages compared to existing methods: simplicity and greenness of sample preparation, use of core-shell column and short analysis time. Conclusion: The results of this study indicate that the combination of dilute and shoot approach and core-shell column can be regarded as an advantageous application for the fast determination of terbinafine in urine.


2018 ◽  
Vol 34 (3) ◽  
pp. 41
Author(s):  
Rogério Adelino De Sousa ◽  
Éder Tadeu Gomes Cavalheiro

A titrimetric procedure for the determination of minoxidil using KMnO4 as oxidizing agent is described. The best conditions were optimized considering the H2SO4, KMnO4 and minoxidil concentrations, the temperature of the system and the order of addition of the reactants. The method was applied to commercial samples and compared with the results from a standard chromatographic procedure. Recoveries from 94.5 to 95.2 % were observed depending on the sample. Comparison with the chromatographic procedure reveled relative errors of -1.00 to – 5.26 %. The method was relatively fast, easy to perform and can be a low cost alternative for pharmaceutical samples in which minoxidil concentration is relatively high.


1955 ◽  
Vol 18 (4) ◽  
pp. 374-378
Author(s):  
Mogens Sprechler

SUMMARY Since 1949 about 10,000 urinary corticoid analyses have been performed routinely in our laboratory. The method used for this purpose was described in 1950 (Sprechler). We determine the corticoids which can be extracted from the urine with chloroform immediately after acidification to pH 1. The extract is washed with sodium hydroxide and water, a Girard separation is performed, and finally the reducing power of the ketonic fraction is measured by means of the phosphomolybdic acid reagent reaction. During the last few years two other chemical reactions have been used for comparison: The formaldehyde and the Porter-Silber method. After a thorough examination of the above methods a standard technique was followed. In the formaldehyde method a microdiffusion in a Conway unit was used instead of distillation of the formaldehyde following the oxidation with periodic acid. The calibration curve was corrected for loss of material by taking the standard doses of DOC through all the procedures of the method. A micromodification of the Porter-Silber method was chosen. Furthermore attempts were made to determine how specific the chromatographic procedure is in the determination of steroids in urinary extracts. For this purpose the Florisil column was used, and the technique described by Nelson & Samuels was followed. Finally we have investigated the glucuronide-bound corticoids in urine in a smaller series of objects.


Author(s):  
V. M. Borishansky ◽  
A.A. Andreevsky ◽  
Mikhail Ya. Belenkiy ◽  
G.S Bykov ◽  
Mikhail Gotovskii ◽  
...  
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