scholarly journals A Capillary Zone Electrophoretic Method for Simultaneous Determination of Seven Drugs in Pharmaceuticals and in Human Urine

2009 ◽  
Vol 92 (5) ◽  
pp. 1382-1389 ◽  
Author(s):  
Amber R Solangi ◽  
Muhammad I Bhanger ◽  
Saima Q Memon ◽  
Muhammad Y Khuhawar ◽  
Arfana Mallah

Abstract A simple, sensitive, and novel method has been developed and validated for the separation and simultaneous quantitation of seven structurally different drugspipemidic acid and ofloxacin quinolone antibiotics, pseudoephedrine decongestant, piroxicam anti-inflammatory, thiamin, pyridoxine, and cobalaminin a mixture by capillary zone electrophoresis. Factors affecting the separation were pH, concentration of buffer, and applied voltage. Separation was carried out in <9 min with a 50 mM sodium tetraborate buffer, pH 10, and an applied voltage of 30 kV in an uncoated silica capillary tube. The carrier electrolyte gave baseline separation with good resolution, reproducibility, and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, and the lower LODs were within the range of 15 g/mL. Detection was performed by UV absorbance at 230 nm. The method was validated for the analysis of drugs in pharmaceutical preparations and in urine samples with RSD of 0.52.4 and recovery of >99.

2010 ◽  
Vol 93 (5) ◽  
pp. 1410-1415 ◽  
Author(s):  
Juan Chen ◽  
Li Chen ◽  
Hong-Li Zhang ◽  
Yan-Ping Shi

Abstract A capillary zone electrophoretic method has been developed for the determination of four coumarinsskimmin, scopolin, scopoletin, and umbelliferonein Saussurea superba with UV detection at 254 nm. The capillary temperature was kept constant at 25°C. Effects of buffer pH, electrolyte concentration, organic modifier, and applied voltage on migration behavior were studied systematically. The optimum conditions for separation were achieved by using 30 mM borate buffer at pH 9.02 containing 15% (v/v) methanol as the electrolyte and 25 kV as the applied voltage. For all analytes a good linear regression relationship (r >0.999) was obtained between peak area and concentration over a relatively wide range. The method was validated for repeatability, precision, and accuracy. The validated method was successfully applied to the simultaneous determination of the four analytes in S. superba.


2008 ◽  
Vol 6 (2) ◽  
pp. 222-228 ◽  
Author(s):  
Sheikha Al-Ghannam ◽  
Abeer Al-Olyan

AbstractA simple and highly sensitive spectrofluorometric method was developed for the determination of some 1,4-dihydropyridine compounds namely, nicardipine, nifedipine and isradipine in pharmaceutical preparations and biological fluids. The method is based on the reduction of nicardipine, nifedipine and isradipine with Zn/HCl and measuring the fluorescence intensity obtained (λem/λex) at 460/364, 450/393 and 446/360 nm, respectively. The factors affecting the development of the fluorophore and its stability were studied and optimized. The effect of some surfactants such as β-cyclodextrin (βCD), carboxymethylcelullose (CMC), sodium dodecyl sulphate (SDS) and triton X-100, on the fluorescence intensity was studied. The fluorescence intensity-concentration plots of nicardipine, nifedipine and isradipine were rectilinear over the ranges 0.4–6.0, 0.2–4.0 and 0.1–9.0 μg ml−1 with detection limits of 0.0028, 0.017 and 0.016 μg ml−1, respectively. The proposed method was successfully applied to commercial tablets containing the compounds; the percentage recovery agreed well with those obtained using the official methods. The method was further extended to the in vitro determination of the compounds in spiked human plasma and urine samples. A proposal of the reduction reaction pathway was postulated.


2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.


2013 ◽  
Vol 5 (8) ◽  
pp. 2126 ◽  
Author(s):  
Carine Viana ◽  
Marlise Ferreira ◽  
Cláudia S. Romero ◽  
Mariana R. Bortoluzzi ◽  
Fernanda O. Lima ◽  
...  

2015 ◽  
Vol 1 (2) ◽  
pp. 11 ◽  
Author(s):  
Safwan Mohammad Fraihat

Two spectrophotometric methods were developed for the determination Tadalafil in pharmaceutical preparations. The methods are based on the oxidation reaction with known excess amount of Ce(IV) and estimation of the unreacted amount using Indigo carmine dye (Method A) and in Methylene blue dye  (Method B). the factors affecting the reaction conditions were studied and the absorbance of absorbance of the oxidation reaction products were monitored at 610 and 600 nm for methods A and B respectively. Beer's law is obeyed in the concentration ranges 11 to 50 and 10 to 55 ppm, the limits of detection and quantification are reported. The proposed method was applied to the determination of the drug in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise and reproducible as the official methods. The validity of method was established by recovery studies with satisfactory results.


2016 ◽  
Vol 52 (2) ◽  
pp. 281-286 ◽  
Author(s):  
Gabriel Hancu ◽  
Anamaria Neacşu ◽  
Lajos Attila Papp ◽  
Adriana Ciurba

ABSTRACT Clavulanic acid enhances the antibacterial spectrum of amoxicillin by rendering most β-lactamase producing isolates susceptible to the drug. A fast, simple and efficient capillary electrophoresis method was developed for the simultaneous determination of amoxicillin and clavulanic acid from complex mixtures. Using a 25 mM sodium tetraborate as background electrolyte at a pH of 9.30, + 25 kV applied voltage, 25 °C system temperature, UV determination at 230 nm; we succeeded in simultaneous separation of amoxicillin and clavulanic acid in approximately 2 minutes. The analytical performance of the method was evaluated in terms of reproducibility, precision, accuracy, and linearity. The optimized analytical method was applied for the determination of the two analytes from combined commercial pharmaceutical preparations. This CE method is fast, inexpensive, efficient, and environmentally friendly when compared with the more frequently used high performance liquid chromatography methods described in the literature.


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