scholarly journals Validation of a Novel Potentiometric Method Based on a Polymeric PVC Membrane Sensor Integrated with Tailored Receptors for the Antileukemia Drug Cytarabine

Polymers ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 1343 ◽  
Author(s):  
Ayman H. Kamel ◽  
Abd El-Galil E. Amr ◽  
Nashwa H. Ashmawy ◽  
Hoda R. Galal ◽  
Abdulrahman A. Almehizia ◽  
...  

A simple, rapid and easy method is proposed for the detection of a cytostatic therapeutic drug, cytarabine, in real samples. The method is based on potentiometric transduction using prepared and characterized new ion-selective electrodes for cytarabine. The electrodes were integrated with novel man-tailored imprinted polymers and used as a sensory element for recognition. The electrodes revealed a remarkable potentiometric response for cytarabine over the linearity range 1.0 × 10−6–1.0 × 10−3 M at pH 2.8–4 with a detection limit of 5.5 × 10−7 M. The potentiometric response was near-Nernstian, with average slopes of 52.3 ± 1.2 mV/decade. The effect of lipophilic salts and plasticizer types on the potentiometric response was also examined. The electrodes exhibited an enhanced selectivity towards cytarabine over various foreign common ions. Validation and verification of the presented assay method are demonstrated by evaluating the method ruggedness and calculating the detection limit, range of linearity, accuracy (trueness), precision, repeatability (within-day) and reproducibility (between-days). The proposed ion-selective electrodes revealed good performance characteristics and possible application of these electrodes for cytarabine monitoring in different matrices. The electrodes are successfully applied to cytarabine determination in spiked biological fluid samples and in pharmaceutical formulations.

Chemosensors ◽  
2020 ◽  
Vol 9 (1) ◽  
pp. 4
Author(s):  
Ville Yrjänä ◽  
Indrek Saar ◽  
Mihkel Ilisson ◽  
Sandip A. Kadam ◽  
Ivo Leito ◽  
...  

Solid-contact ion-selective electrodes with carbazole-derived ionophores were prepared. They were characterized as acetate sensors, but can be used to determine a number of carboxylates. The potentiometric response characteristics (slope, detection limit, selectivity, and pH sensitivity) of sensors prepared with different membrane compositions (ionophore, ionophore concentration, anion exchanger concentration, and plasticizer) were evaluated. The results show that for the macrocyclic ionophores, a larger cavity provided better selectivity. The sensors exhibited modest selectivity for acetate but good selectivity for benzoate. The carbazole-derived ionophores effectively decreased the interference from lipophilic anions, such as bromide, nitrate, iodide, and thiocyanate. The selectivity, detection limit, and linear range were improved by choosing a suitable plasticizer and by reducing the ionophore and anion exchanger concentrations. The influence of the electrode body’s material upon the composition of the plasticized poly(vinyl chloride) membrane, and thus also upon the sensor characteristics, was also studied. The choice of materials for the electrode body significantly affected the characteristics of the sensors.


2009 ◽  
Vol 2009 ◽  
pp. 1-7 ◽  
Author(s):  
Hassan Arida ◽  
Mona Ahmed ◽  
Abdallah Ali

The fabrication and electrochemical evaluation of two PVC membrane-based Ion-Selective electrodes responsive for ramipril drug have been proposed. The sensitive membranes were prepared using ramipril-phosphomolibdate and ramipril-tetraphenylborate ion-pair complexes as electroactive sensing materials in plasticized PVC support. The electrodes based on these materials provide near-Nernestian response (sensitivity of53±0.5–54±0.5 mV/concentration decade) covering the concentration range of1.0×10-2–1.0×10-5 molL−1with a detection limit of3.0×10-6–4.0×10-6 molL−1. The suggested electrodes have been successfully used in the determination of ramipril drug in some pharmaceutical formulations using direct potentiometry with average recovery of >96% and mean standard deviation of <3% (n=5).


2017 ◽  
Vol 100 (5) ◽  
pp. 1414-1419
Author(s):  
Nesreen Khamees ◽  
Tagreed Abdel-Fattah Mohamed ◽  
Abeer Rashad Derar ◽  
Azza Aziz

Abstract All-solid-state, polyvinyl chloride (PVC) membrane, and carbon paste potentiometric ion-selective electrodes (ISEs) were proposed for the determination of donepezil hydrochloride (DON) in the drug substance and a pharmaceutical formulation. The potentiometric response toward DON was based on the existence ofdonepezil-tetraphenyl borate (DON-TPB) in a PVC membrane or a carbon paste in the presence of dioctylphthalate. In contrast, the solid-state electrode was prepared by direct incorporation of DON-TPB into a commercial nail varnish without external additives. The electrodes exhibited Nernstian slopes of 55.0, 57.0, and 53.0 mV/decade over the concentration ranges of 1 × 10−5 to 1 × 10−3, 1 × 10−4 to 10−2, and 1 × 10−4 to 5 × 10−3 for the solid-state, PVC membrane, and carbon paste electrodes, respectively. The response of the electrodes is independent of pH in the range of 2–≤8. The electrodes showed good selectivity for DON with respect to a number of inorganic cations and amino acids. The electrodes were used for the determination of DON in pure solution and in pharmaceutical tablets with high accuracy (±2%) and precision (RSD ≤2%). The solid-state electrode is simple, economical, and rapid when compared to the PVC membrane and carbon paste electrodes.


Author(s):  
Vishal N Kushare ◽  
Sachin S Kushare

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for Ozagrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Ozagrel (Rf value of 0.40 ± 0.010). Densitometric analysis of Ozagrel was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Ozagrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Ozagrel in pharmaceutical formulations. The limits of detection and quantitation were 4.069 and 12.332 ng/spot, respectively by height. Ozagrel was subjected to acid and alkali hydrolysis, oxidation, photochemical and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and heat conditions. This indicates that the drug is susceptible to acid, base hydrolysis, oxidation and heat. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Ozagrel in bulk drug and tablet formulation.


Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  


2020 ◽  
Vol 16 (7) ◽  
pp. 967-975
Author(s):  
Abubakr M. Idris

Methods: Sequential injection chromatography (SIC) with monolithic column has been proposed with potential benefits for separation and quantification. Objective: To utilize SIC to develop a new assay method for the separation and quantification of some phenothiazines (promethazine, chlorpromazine and perphenazine) in human urine and synthetic pharmaceutical formulations. Methods: The 32 full-factorial design was adopted to study the effect of mobile phase composition on separation efficiency, retention time, peak height and baseline. The separation was conducted on a C18 monolithic column (100 × 4.6 mm) using a mobile phase composition of phosphate: acetonitrile:methanol (60:28:12) at pH 4.0. The detection was carried out using a miniaturized fiber optic spectrometer at 250 nm. Results: Satisfactory analytical features, including number of theoretical plates (1809-6232), peak symmetry (1.0-1.3), recovery (95.5-99.1% in pharmaceutical formulations and 91.6-94.7% in urine), intra-day precision (0.36-1.60% for pharmaceutical formulation and 2.96-3.67 for urine), inter-day precision (1.47-2.28% for pharmaceutical formulation), limits of detection (0.23-0.88 μg/ml) and limits of quantification (0.77-2.90 μg/ml), were obtained. Conclusion: The remarkable advantages of the proposed SIC method are the inexpensiveness in terms of instrumentation and reagent consumption.


2020 ◽  
Vol 16 (2) ◽  
pp. 168-175 ◽  
Author(s):  
Merve Tumur ◽  
Gulsah Saydan Kanberoglu ◽  
Fatih Coldur

Background: Cysteamine is used as an orphan drug in the treatment of cystinosis to prevent long-term cystine accumulation in lysosomes. Dosing in cysteamine treatment is extremely important and overdose may cause some side effects. Up to now, various analytical methods have been used for cysteamine determination. Many of these methods require sophisticated instruments, expert operators, time-consuming measurement procedures and manipulation steps, expensive supplies and long analysis time. Aims and Objective: The present study deals with the development of a potentiometric PVC-membrane cysteamine-selective electrode based on an ion-pair of cysteamine and its application in a pharmaceutical formulation. Methods: Cysteamine (Cys)-Phosphomolybdate (PM) ion-pair was synthesized by mixing the equal volumes of 10-2 M Cysteamine HCl and sodium phosphomolybdate aqueous solutions. The obtained precipitate was used as ionophore in the structure of PVC-membrane. Results and Discussion: The electrode exhibited a linear response in the concentration range of 1.0×10- 1-1.0×10-5 M cysteamine with a slope of 51,7 mV per decade and detection limit of 1.0×10-5 M. The potentiometric response of the electrode was very rapid (5 s), adequately repeatable, stable and selective. pH working range and life-time of the electrode were also determined as 3.0-7.0 and 25 days, respectively. Conclusion: A PVC-membrane cysteamine selective electrode was easily prepared. Cysteamine determination in a pharmaceutical formulation was performed. Analysis results indicated that it can be successfully used in drug quality control laboratories for routine analysis of cysteamine in pharmaceutical preparations alternative to more sophisticated, expensive and time-consuming analytical methods.


2020 ◽  
Vol 40 (10) ◽  
pp. 842-847
Author(s):  
Shankar Suman ◽  
Ram Singh

AbstractA new poly (vinyl chloride) (PVC) membrane electrode using 2-benzoylpyridine semicarbazone as membrane carrier with dioctylphthalate as plasticizer and sodium tetraphenylborate (NaTBP) as anion excluder has been fabricated and investigated as Zn(II)-selective electrode. Best potential response is observed for the composition PVC 30%, plasticizer 58%, NaTBP 8% and ionophore 4% (w/w). The sensor showed a linear stable response over a concentration range of 1.0 × 10−2–4.56 × 10−6 M with a detection limit of 2.28 × 10−6 M and a response time <10 s. The electrode can be used for at least six months without any divergence in potential.


Sensors ◽  
2021 ◽  
Vol 21 (9) ◽  
pp. 3150
Author(s):  
Fatehy M. Abdel-Haleem ◽  
Sonia Mahmoud ◽  
Nour Eldin T. Abdel-Ghani ◽  
Rasha Mohamed El Nashar ◽  
Mikhael Bechelany ◽  
...  

Levofloxacin (LF) is a medically important antibiotic drug that is used to treat a variety of bacterial infections. In this study, three highly sensitive and selective carbon paste electrodes (CPEs) were fabricated for potentiometric determination of the LF drug: (i) CPEs filled with carbon paste (referred to as CPE); (ii) CPE coated (drop-casted) with ion-selective PVC membrane (referred to as C-CPE); (iii) CPE filled with carbon paste modified with a plasticizer (PVC/cyclohexanone) (referenced as P-CPE). The CPE was formulated from graphite (Gr, 44.0%) and reduced graphene oxide (rGO, 3.0%) as the carbon source, tricresyl phosphate (TCP, 47.0%) as the plasticizer; sodium tetrakis[3,5-bis(trifluoromethyl)phenyl] borate (St-TFPMB, 1.0%) as the ion exchanger; and levofloxacinium-tetraphenylborate (LF-TPB, 5.0%) as the lipophilic ion pair. It showed a sub-Nernstian slope of 49.3 mV decade−1 within the LF concentration range 1.0 × 10−2 M to 1.0 × 10−5 M, with a detection limit of 1.0 × 10−5 M. The PVC coated electrode (C-CPE) showed improved sensitivity (in terms of slope, equal to 50.2 mV decade−1) compared to CPEs. After the incorporation of PVC paste on the modified CPE (P-CPE), the sensitivity increased at 53.5 mV decade−1, indicating such improvement. The selectivity coefficient (log KLF2+,Fe+3pot.) against different interfering species (Na+, K+, NH4+, Ca2+, Al3+, Fe3+, Glycine, Glucose, Maltose, Lactose) were significantly improved by one to three orders of magnitudes in the case of C-CPE and P-CPE, compared to CPEs. The modification with the PVC membrane coating significantly improved the response time and solubility of the LF-TPB within the electrode matrix and increased the lifetime. The constructed sensors were successfully applied for LF determination in pharmaceutical preparation (Levoxin® 500 mg), spiked urine, and serum samples with high accuracy and precision.


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