scholarly journals A Chemosensor Based on Gold Nanoparticles and Dithiothreitol (DTT) for Acrylamide Electroanalysis

Nanomaterials ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 2610
Author(s):  
Shahenvaz Alam ◽  
Shine Augustine ◽  
Tarun Narayan ◽  
John H. T. Luong ◽  
Bansi Dhar Malhotra ◽  
...  
Keyword(s):  
Surface Roughness ◽  
Gold Nanoparticles ◽  
High Performance ◽  
Gold Electrode ◽  
Limit Of Detection ◽  
Active Surface ◽  
Detection Sensitivity ◽  
Active Surface Area ◽  
Surface Plasmon Resonance Analysis ◽  
Limit Of Quantitation

Rapid and simple electroanalysis of acrylamide (ACR) was feasible by a gold electrode modified with gold nanoparticles (AuNPs) and dithiothreitol (DTT) with enhanced detection sensitivity and selectivity. The roughness of bare gold (Au) increased from 0.03 μm to 0.04 μm when it was decorated with AuNPs. The self-assembly between DTT and AuNPs resulted in a surface roughness of 0.09 μm. The DTT oxidation occurred at +0.92 V. The Au/AuNPs/DTT surface exhibited a surface roughness of 0.24 μm after its exposure to ACR with repeated analysis. SEM imaging illustrated the formation of a polymer layer on the Au/AuNPs/DTT surface. Surface plasmon resonance analysis confirmed the presence of AuNPs and DTT on the gold electrode and the binding of ACR to the electrode’s active surface area. The peak area obtained by differential pulse voltammetry was inversely proportional to the ACR concentrations. The limit of detection (LOD) and the limit of quantitation (LOQ) were estimated to be 3.11 × 10−9 M and 1 × 10−8 M, respectively, with wide linearity ranging from 1 × 10−8 M to 1 × 10−3 M. The estimated levels of ACR in potato chips and coffee samples by the sensor were in agreement with those of high-performance liquid chromatography.

Validated Stability Indicating HPTLC Method for the Estimation of Amoxapine in Different Stress Conditions

2019 ◽  
Vol 15 (3) ◽  
pp. 273-279
Author(s):  
Shweta G. Rangari ◽  
Nishikant A. Raut ◽  
Pradip W. Dhore
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Analysis Data ◽  
Peak Height ◽  
Good Resolution ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Wide Range ◽  
Hptlc Method

Background:The unstable and/or toxic degradation products may form due to degradation of drug which results into loss of therapeutic activity and lead to life threatening condition. Hence, it is important to establish the stability characteristics of drug in various conditions such as in temperature, light, oxidising agent and susceptibility across a wide range of pH values.Introduction:The aim of the proposed study was to develop simple, sensitive and economic stability indicating high performance thin layer chromatography (HPTLC) method for the quantification of Amoxapine in the presence of degradation products.Methods:Amoxapine and its degraded products were separated on precoated silica gel 60F254 TLC plates by using mobile phase comprising of methanol: toluene: ammonium acetate (6:3:1, v/v/v). The densitometric evaluation was carried out at 320 nm in reflectance/absorbance mode. The degradation products obtained as per ICH guidelines under acidic, basic and oxidative conditions have different Rf values 0.12, 0.26 and 0.6 indicating good resolution from each other and pure drug with Rf: 0.47. Amoxapine was found to be stable under neutral, thermal and photo conditions.Results:The method was validated as per ICH Q2 (R1) guidelines in terms of accuracy, precision, ruggedness, robustness and linearity. A good linear relationship between concentration and response (peak area and peak height) over the range of 80 ng/spot to 720 ng/spot was observed from regression analysis data showing correlation coefficient 0.991 and 0.994 for area and height, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) for area were found to be 1.176 ng/mL and 3.565 ng/mL, whereas for height, 50.063 ng/mL and 151.707 ng/mL respectively.Conclusion:The statistical analysis confirmed the accuracy, precision and selectivity of the proposed method which can be effectively used for the analysis of amoxapine in the presence of degradation products.

scholarly journals High-Performance Lead-Acid Batteries Enabled by Pb and PbO2 Nanostructured Electrodes: Effect of Operating Temperature

2021 ◽  
Vol 11 (14) ◽  
pp. 6357
Author(s):  
Roberto Luigi Oliveri ◽  
Maria Grazia Insinga ◽  
Simone Pisana ◽  
Bernardo Patella ◽  
Giuseppe Aiello ◽  
...  
Keyword(s):  
High Performance ◽  
Active Material ◽  
Active Surface ◽  
Effect Of Temperature ◽  
Active Surface Area ◽  
Polycarbonate Membrane ◽  
Nanostructured Electrodes ◽  
Lead Acid Batteries ◽  
Improved Stability ◽  
Lead Acid

Lead-acid batteries are now widely used for energy storage, as result of an established and reliable technology. In the last decade, several studies have been carried out to improve the performance of this type of batteries, with the main objective to replace the conventional plates with innovative electrodes with improved stability, increased capacity and a larger active surface. Such studies ultimately aim to improve the kinetics of electrochemical conversion reactions at the electrode-solution interface and to guarantee a good electrical continuity during the repeated charge/discharge cycles. To achieve these objectives, our contribution focuses on the employment of nanostructured electrodes. In particular, we have obtained nanostructured electrodes in Pb and PbO2 through electrosynthesis in a template consisting of a nanoporous polycarbonate membrane. These electrodes are characterized by a wider active surface area, which allows for a better use of the active material, and for a consequent increased specific energy compared to traditional batteries. In this research, the performance of lead-acid batteries with nanostructured electrodes was studied at 10 C at temperatures of 25, −20 and 40 °C in order to evaluate the efficiency and the effect of temperature on electrode morphology. The batteries were assembled using both nanostructured electrodes and an AGM-type separator used in commercial batteries.

Hollow structure engineering of FeCo alloy nanoparticles electrospun in nitrogen-doped carbon enables high performance flexible all-solid-state zinc–air batteries

2020 ◽  
Vol 4 (4) ◽  
pp. 1747-1753 ◽  
Author(s):  
Yuanyuan Ma ◽  
Wenjie Zang ◽  
Afriyanti Sumboja ◽  
Lu Mao ◽  
Ximeng Liu ◽  
...  
Keyword(s):  
Active Sites ◽  
High Performance ◽  
Hollow Structure ◽  
Active Surface ◽  
Oxygen Electrode ◽  
Active Surface Area ◽  
Active Components ◽  
Nitrogen Doped Carbon ◽  
Structure Engineering ◽  
Kinetics Of

Hollow structuring of active components is an effective strategy to improve the kinetics of oxygen electrode catalysts, arising from the increased the active surface area, the defects on the exposed surface, and the accessible active sites.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

Stability Indicating HPTLC Method for Simultaneous Determination of Amlodipine Besylate and Lisinopril in Combined Dose Tablet Formulation

2021 ◽  
pp. 6250-6256
Author(s):  
Sagar B. Wankhede ◽  
Deepak S. Khobragade ◽  
Sukeshini B. Lote ◽  
S. Patil
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Cost Effective ◽  
Tablet Formulation ◽  
Simultaneous Estimation ◽  
Amlodipine Besylate ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Dose Tablet

A combined dose tablet formulation containing Amlodipine besylate and Lisinopril is used for the treatment of essential hypertension. The present study reports development and validation of stability indicating high performance thin layer chromatographic method for simultaneous estimation of these drugs in combined dose tablet formulation. The two drugs were satisfactorily resolved on aluminum plates precoated with silica gel 60F254 using n-butanol : methanol: ammonia (4:4:1 v/v/v) as mobile phase. The Rf value for lisinopril and amlodipine besylate were 0.27±0.02 and 0.62±0.02, respectively. Densitometric evaluation of the separated bands was performed at 215nm. The calibration curves for lisinopril and amlodipine besylate were found to be linear in the concentration range of 1000-6000ng/band. The method was validated as per ICH guidelines for accuracy, precision, robustness, specificity, limit of detection and limit of quantitation. Statistical analysis proves that the method is suitable for simultaneous analysis of Lisinopril and Amlodipine besylate in pharmaceutical formulation without any interference from the excipients/degradant. The developed method offers several advantages such as sensitive, rapid, cost effective and less time consuming as compared to the reported methods. As the method could effectively separate the drugs from its degradation products, it can be employed as a stability indicating method.

Performance evaluation of an Indoxyl Sulfate Assay Kit “NIPRO”

2019 ◽  
Vol 57 (11) ◽  
pp. 1770-1776 ◽  
Author(s):  
Yuki Fushimi ◽  
Junko Tatebe ◽  
Yuko Okuda ◽  
Toshiaki Ishii ◽  
Shinji Ujiie ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Cardiorenal Syndrome ◽  
Indoxyl Sulfate ◽  
Analytical Performance ◽  
Limit Of Quantitation ◽  
Interference Test ◽  
Interference Tests ◽  
The Relationship ◽  
Method R

Abstract Background The relationship between renal disease and cardiovascular disease (CVD) is currently known as cardiorenal syndrome. Indoxyl sulfate (IS) is one of the uremic toxins that accelerates the progression of cardiorenal syndrome. This report presents a new method for measuring IS in a simpler way. Methods We evaluated the analytical performance of an IS Assay Kit “NIPRO” loaded on LABOSPECT 008. The evaluated analytical performances included accuracy, precision, dilution linearity, limit of detection (LOD), limit of quantitation (LOQ), recovery test, interference test and comparison against assays performed by high-performance liquid chromatography (HPLC). Results Total precision showed a <5.3% coefficient of variation at IS concentrations of 3.57–277.73 μmol/L, and satisfactory results were observed in the dilution linearity, LOD, LOQ, recovery and interference tests. The IS Assay Kit “NIPRO” showed a high correlation with the HPLC conventional method (r = 0.993). Conclusions The IS Assay Kit “NIPRO” demonstrated satisfactory analytical performance, and this suggests it could shortly become another common method to measure circulating IS.

Metallic Film Modified Screen-Printed Carbon Electrode for Determination of 17α-Methyltestosterone

2019 ◽  
Vol 824 ◽  
pp. 182-189
Author(s):  
Chim Math ◽  
Wijitar Dungchai ◽  
Sudtida Pliankarom Thanasupsin
Keyword(s):  
Modified Electrode ◽  
Limit Of Detection ◽  
Diffusion Mechanism ◽  
Modified Electrodes ◽  
Active Surface ◽  
Deposition Potential ◽  
Active Surface Area ◽  
Male Population ◽  
Screen Printed Carbon Electrode ◽  
Screen Printed

17α-methyltestosterone (MT) is a synthetic androgen. It is used widely for inducing an all-male population of Nile tilapia (Oreochromis niloticus). In this work, the detection of MT was conducted using screen-printed carbon electrodes (SPCE). These were a bare electrode, a bismuth modified electrode (Bi-SPCE) and an antimony modified electrode (Sb-SPCE). The successful electrode modification was confirmed by scanning electron microscopy. The electroanalytical performance of the SPCE modified electrodes for MT detection was examined by cyclic voltammetry. The highest active surface area of 1.073x10-4 cm2 was obtained on Sb-SPCE. This indicates that Sb-SPCE can enhance the sensitivity of MT detection better than the bare-SPCE and the Bi-SPCE. The Sb-SPCE showed a linear response for MT concentrations ranging from 2 to 8 mg.L-1. The sensitivity obtained from the slope of a calibration curve was -0.452 mA.mol-1.L-1 in a Britton-Robinson buffer pH 4.0 containing Sb 16 mg.L-1 with deposition potential and deposition time of 1 V and 90 seconds, respectively. A linear relationship between the square root of the scan rate and the peak current revealed that mass transfer of MT to the electrode was driven by a diffusion mechanism. The limit of detection was found to be 1 mg.L-1.

scholarly journals Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were &lt;0.46 and &lt;0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

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