scholarly journals Determination of Atorvastatin with Voltammetric Sensors Based on Nanomaterials

Inventions ◽  
2021 ◽  
Vol 6 (3) ◽  
pp. 57
Author(s):  
Ramona Oana Gunache (Roșca) ◽  
Alexandra Virginia Bounegru ◽  
Constantin Apetrei
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Products ◽  
Spectrometric Method ◽  
Background Current ◽  
Limit Of Quantification ◽  
Voltammetric Sensors ◽  
Printed Sensors ◽  
Lower Background

This paper presents an accurate and fast electrochemical method for atorvastatin determination in pharmaceutical products. Two screen-printed sensors, one—carbon based (SPCE) and one based on carbon nanotubes and gold nanoparticles (AuNP-CNT/SPCE) were used during the electrochemical analyses. At all experimental stages, cyclic voltammetry was employed, both for the characterization of the sensors and their electrochemical behavior, and for quantitative determinations. AuNP-CNT/SPCE has showed an extended active area, higher intensity peaks, better reversibility and lower background current than the unmodified sensor. For atorvastatin quantification, a calibration curve has been developed within the 1.2–606.25 µM concentration range. A linearity relation between the current of the anodic peak and concentration has been obtained in the range 1.2–53.33 µMfor both sensors. With the AuNP-CNT/SPCE sensor, low values of limit of detection, LOD (1.92 × 10−7 M) and limit of quantification, LOQ (6.39 × 10−7 M) have been obtained, which demonstrates the feasibility of the method of determining atorvastatin from real samples. Atorvastatin amount has been successfully determined from pharmaceutical products using AuNP-CNT/SPCE. The results were similar to the manufacturer’s specifications regarding the dosage per tablet and to the concentrations obtained by applying the FTIR spectrometric method.

scholarly journals Determination of Lisinopril in Pure and Tablet form by Using 2-Hydroxynaphthaldehyde as Derivatizing Reagent

2021 ◽  
Vol 22 (1) ◽  
pp. 115-126
Author(s):  
Zahid Ali Zounr
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Products ◽  
Molar Absorptivity ◽  
Coefficient Of Determination ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Tablet Form ◽  
Derivatizing Reagent ◽  
Derivatization Reaction

An easy, sensitive and accurate spectrophotometric method has been developed for the determination of Lisinopril (LNP) in pure and tablet formulations based on derivatization reaction with 2-hydroxynaphthaldehyde (2HNA). The derivatization reaction was carried out in methanol solvent at pH-5.5 at 95±2C for 15 min. The linear calibration curve was obtained that obeyed the Beer’s law within the concentration range 5-50 μgmL-1 of LNP at 433 nm with a coefficient of determination R²=0.996. The recovery was in the range from 98.25-101.82 with molar absorptivity of drug 9×103 mole-1cm-1. The method was accurate and precise (intra-day variation 0.05-0.97% and inter-day 0.07-1.6%), with limit of detection (LOD) and limit of quantification (LOQ) 0.264 μgmL-1 and 0.8 μgmL-1, respectively. No interferences from the excipients were detected. The method was applied for the rapid analysis of LNP in pharmaceutical products.

scholarly journals Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

2015 ◽  
Vol 51 (4) ◽  
pp. 879-891 ◽  
Author(s):  
Serpil Sevim ◽  
Nevin Erk
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Pharmaceutical Products ◽  
Pharmaceutical Product ◽  
Limit Of Quantification ◽  
First Derivative ◽  
Pramipexole Dihydrochloride

abstract The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC) and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4) and acetonitrile (35:65 by volume). The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL) and limit of quantification (50 ng/mL) were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000). In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method.

scholarly journals Trace Level Determination of Polyether Ionophores in Feed

2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Mervi Rokka ◽  
Marika Jestoi ◽  
Kimmo Peltonen
Keyword(s):  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Spectrometric Method ◽  
Mass Spectrometric Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Feed Control ◽  
Carry Over ◽  
Feed Samples

A liquid chromatography-mass spectrometric method was developed and validated to determine six polyether ionophores (lasalocid sodium, monensin sodium, salinomycin sodium, narasin, maduramicin ammonium alpha, and semduramicin sodium) in feed samples. The method developed was very straightforward, involving extraction with 84% acetonitrile of the coccidiostats from the feed samples and filtration of the raw extract prior to chromatographic analysis. Method validation included the determination of selectivity, linearity, specificity, repeatability, the limit of detection, limit of quantification, decision limit (CCα), detection capability (CCβ), and recovery. Feed samples from the Finnish national feed control programme and suspected carry-over samples from a feed manufacturer were analysed in parallel with an existing liquid chromatography method coupled with ultraviolet detection. All feed control samples were negative in LC-UV, but with the developed MS method, monensin, salinomycin, and narasin were detected at concentrations of <0.025–0.73 mg/kg, <0.025–0.027 mg/kg, and <0.025–1.6 mg/kg, respectively. In suspected carry-over samples after an output of 2.0 tonnes of unmedicated feed in the pelletizer line, the concentrations of monensin, salinomycin, and narasin varied from undetected to 16 mg/kg. In the mixer line, after 3.2 tonnes of unmedicated feed output, the concentrations of monensin, salinomycin, and narasin varied from undetected to 2.4 mg/kg.

scholarly journals Facile Electrochemical Determination of Methotrexate (MTX) Using Glassy Carbon Electrode-Modified with Electronically Disordered NiO Nanostructures

Nanomaterials ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 1266
Author(s):  
Aftab A. Khand ◽  
Saeed A. Lakho ◽  
Aneela Tahira ◽  
Mohd Ubaidullah ◽  
Asma A. Alothman ◽  
...  
Keyword(s):  
Glassy Carbon Electrode ◽  
Glassy Carbon ◽  
Limit Of Detection ◽  
Linear Sweep Voltammetry ◽  
Pharmaceutical Products ◽  
Linear Range ◽  
Carbon Electrode ◽  
Limit Of Quantification ◽  
Recovery Method

Recently, the oxidative behavior of methotrexate (MTX) anticancer drug is highly demanded, due to its side effects on healthy cells, despite being a very challenging task. In this study, we have prepared porous NiO material using sodium sulfate as an electronic disorder reagent by hydrothermal method and found it highly sensitive and selective for the oxidation of MTX. The synthesized NiO nanostructures were characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) techniques. These physical characterizations delineated the porous morphology and cubic crystalline phase of NiO. Different electrochemical approaches have been utilized to determine the MTX concentrations in 0.04 M Britton–Robinson buffer (BRB) at pH 2 using glassy carbon electrode (GCE)-modified with electronically disordered NiO nanostructures. The linear range for MTX using cyclic voltammetry (CV) was found to be from 5 to 30 nM, and the limit of detection (LOD) and limit of quantification (LOQ) were 1.46 nM and 4.86 nM, respectively, whereas the linear range obtained via linear sweep voltammetry (LSV) was estimated as 15–90 nM with LOD and LOQ of 0.819 nM and 2.713 nM, respectively. Additionally, amperometric studies revealed a linear range from 10 to70 nM with LOD and LOQ of 0.1 nM and 1.3 nM, respectively. Importantly, MTX was successfully monitored in pharmaceutical products using the standard recovery method. Thus, the proposed approach for the synthesis of active metal oxide materials could be sued for the determination of other anticancer drugs in real samples and other biomedical applications.

scholarly journals Synthesis and Characterization of GO/ZIF-67 Nanocomposite: Investigation of Catalytic Activity for the Determination of Epinine in the Presence of Dobutamine

Micromachines ◽  
2022 ◽  
Vol 13 (1) ◽  
pp. 88
Author(s):  
Mahboobeh Shahsavari ◽  
Mojtaba Mortazavi ◽  
Somayeh Tajik ◽  
Iran Sheikhshoaie ◽  
Hadi Beitollahi
Keyword(s):  
Limit Of Detection ◽  
Simultaneous Detection ◽  
Differential Pulse ◽  
Screen Printed Electrode ◽  
Limit Of Quantification ◽  
Diffusion Controlled ◽  
Rate Study ◽  
The Stability

In this study, we prepared graphene oxide (GO)/ZIF-67 nanocomposites. Therefore, GO/ZIF-67 nanocomposites were used as a modifier on a screen-printed electrode (GO/ZIF-67/SPE) for studying the electrochemical behavior of epinine in phosphate buffer saline (PBS) at pH 7.0 with voltammetry techniques. The GO/ZIF-67/SPE showed greater electrocatalytic activities than the bare SPE. As a result, the GO/ZIF-67/SPE was utilized for additional electrochemical examinations. The epinine concentration determination was in the range 9.0 × 10−8 M to 5.0 × 10−4 M, and the limit of detection (LOD) as well as the limit of quantification (LOQ) equaled 2.0 and 6.6 nM, respectively. From the scan rate study, the oxidation of epinine was found to be diffusion-controlled, and the simultaneous detection of epinine and dobutamine were well achieved with the differential pulse voltammetric (DPV) technique. Moreover, the stability and reproducibility of epinine at the GO/ZIF-67/SPE was studied, and the use of the GO/ZIF-67/SPE to detect epinine and dobutamine in real samples was furthermore successfully demonstrated.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals Surface-Enhanced Oxidation and Determination of Isothipendyl Hydrochloride at an Electrochemical Sensing Film Constructed by Multiwalled Carbon Nanotubes

2012 ◽  
Vol 2012 ◽  
pp. 1-6
Author(s):  
S. N. Prashanth ◽  
Shankara S. Kalanur ◽  
Nagappa L. Teradal ◽  
J. Seetharamappa
Keyword(s):  
Limit Of Detection ◽  
Biological Fluids ◽  
Differential Pulse ◽  
Electrochemical Sensing ◽  
Good Precision ◽  
Multiwalled Carbon ◽  
Limit Of Quantification ◽  
Surface Enhanced ◽  
Ph Range

The electrochemical behavior of isothipendyl hydrochloride (IPH) was investigated at bare and multiwalled-carbon-nanotube modified glassy carbon electrode (MWCNT-GCE). IPH (55 μM) showed two oxidation peaks in Britton-Robinson (BR) buffer of pH 7.0. The oxidation process of IPH was observed to be irreversible over the pH range of 2.5–9.0. The influence of pH, scan rate, and concentration of the drug on anodic peak was studied. A differential pulse voltammetric method with good precision and accuracy was developed for the determination of IPH in pure and biological fluids. The peak current was found to be linearly dependent on the concentration of IPH in the range of 1.25–55 μM. The values of limit of detection and limit of quantification were noticed to be 0.284 and 0.949 μM, respectively.

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