scholarly journals Development of Flow Injection Spectrophotometric Method for 1-Napthylthiourea Using Sodium Nitrite and Sulphanilic Acid Diazotization Reaction

2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Muhammad Asghar ◽  
Mohammad Yaqoob ◽  
Sami Ullah ◽  
Samar Ali ◽  
Nusrat Munawar ◽  
...  
Keyword(s):  
Flow Injection ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Calibration Equation ◽  
Sulphanilic Acid ◽  
Paired Student ◽  
Relative Standard ◽  
Hydrolysis Of

A simple spectrophotometric method in conjunction with flow injection analysis is developed for the quantitative analysis of 1-napthylthiourea (ANTU). The reaction is based on the alkaline hydrolysis of ANTU to 1-naphthylamine at 30°C, coupled with diazotized sulphanilic acid resulting in 4-(sulphophenylazo)-1-naphthylamine which is monitored at 495 nm. The limit of detection (S/N = 3) is 0.01 mg/L with a sampling throughput of 45/h. The method is linear over the range of 0.05–120 mg/L (R2=0.9995,n=7), with calibration equation y = 0.031x−0.018 (y = absorbance; x = mg/L) and relative standard deviation (n=3) 1.8–3.6%. Experimental variables are optimised, and the interfering effects of different pesticides, organic compounds, cations, and anions at environmentally relevant concentrations are investigated. The analysis of ANTU in spiked water samples is extracted with solid phase procedure using disposable Sep-Pak C18 cartridges, and the recovery was 93 ± 1.9–110 ± 3.0%. The results of the proposed method are compared with the HPLC method by applying the F-test and paired Student t-test at 95% confidence level.

scholarly journals Development of a kinetic spectrophotometric method for insecticide diflubenzuron determination in water and baby food samples

2018 ◽  
Vol 72 (5) ◽  
pp. 305-314 ◽  
Author(s):  
Emilija Pecev-Marinkovic ◽  
Zora Grahovac ◽  
Aleksandra Pavlovic ◽  
Snezana Tosic ◽  
Ivana Rasic-Misic ◽  
...  
Keyword(s):  
Spectrophotometric Method ◽  
Solid Phase ◽  
Kinetic Method ◽  
Inhibitory Effect ◽  
Food Samples ◽  
Hplc Method ◽  
Baby Food ◽  
Relative Standard ◽  
Concentration Interval ◽  
Kinetic Spectrophotometric

A kinetic spectrophotometric method for determining residues of insecticide diflubenzuron 1(4-chlorphenyl)-3-(2,6-diflubenzoyl)urea (DFB) has been developed and validated. Kinetic method was based on the inhibitory effect of DFB on the oxidation reaction of sulfanilic acid (SA) by hydrogen peroxide in the presence of Co2+ ions in a phosphate buffer, which was monitored at 370 nm. DFB can be measured in the concentration interval 0.102 ? 3.40 ?g mL-1 and 3.40 ? 23.80 ?g mL-1. The detection and quantification limits of the method were calculated according to the 3? criteria and found to be 0.077 ?g mL-1 and 0.254 ?g Ml-1, respectively. The relative standard deviations for five replicate determinations of 0.102, 1.70 and 3.40 ?g mL-1 DFB were 2.08, 1.22 and 1.21 %, respectively, for the first concentration interval, and the recovery percentage values were from 94.12 to 97.35 %. HPLC method was used as a parallel method to verify results of the kinetic method. The kinetic method was successfully applied to determine diflubenzuron concentrations in spiked water and baby food samples after solid phase extraction of the samples. The F and t values at 95% confidence level are lower than the theoretical ones, confirming agreement of the developed and the HPLC method.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

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 Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals The Development of a New Kinetic Spectrophotometric Method for the Determination of Vanadium(V) Based on its Catalytic Effect on the Oxidation of Malachite Green Oxalate by Bromate in Acidic and Micellar Medium

2010 ◽  
Vol 7 (4) ◽  
pp. 1612-1620 ◽  
Author(s):  
M. Keyvanfard ◽  
N. Abedi
Keyword(s):  
Malachite Green ◽  
Spectrophotometric Method ◽  
Catalytic Effect ◽  
Limit Of Detection ◽  
Fixed Time ◽  
Micellar Medium ◽  
Relative Standard ◽  
Kinetic Spectrophotometric ◽  
Malachite Green Oxalate

A new, simple, sensitive and selective kinetic spectrophotometric method was developed for the determination of ultra trace amounts of vanadium(V). The method is based on the catalytic effect of vanadium(V) on the oxidation of malachite green oxalate (MG) by bromate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of malachite green oxalate (MG) at 625 nm with a fixed-time method. The decrease in the absorbance of MG is proportional to the concentration of vanadium(V) in the range of 1-100 ng/mL with a fixed time of 0.5-2 min from the initiation of the reaction. The limit of detection is 0.71 ng/mL of vanadium(V). The relative standard deviation for the determination of 5, 30, 50 ng/mL of vanadium(V) was2.5% 2.6%, 2.4% and respectively. The method was applied to the determination of vanadium(V) in water samples.

Determination of Bendiocarb Insecticide by Reverse Flow Injection Analysis Using a Solid-Phase Reactor Containing Micro PbO2, Nano PbO2 and Grafted SiO2 - PbO2 Immobilized

2020 ◽  
Vol 42 (1) ◽  
pp. 31-31
Author(s):  
Malik H Alaloosh Alamri Malik H Alaloosh Alamri ◽  
Sadeem Subhi Abed and Abdulkareem M A Alsammarraie Sadeem Subhi Abed and Abdulkareem M A Alsammarraie
Keyword(s):  
Flow Injection ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reverse Flow ◽  
Blue Color ◽  
Wide Range ◽  
Solid Phase Reactor ◽  
Grafted Nanoparticles ◽  
Reverse Flow Injection

Bendiocarb (BEN) is an acutely toxic carbamate insecticide which used in public places and agriculture, it is also effective against a wide range of nuisance and disease vector insects. A new rapid and sensitive reverse flow injection spectrophotometric procedure coupled with on-line solid-phase reactor is designed in this article for the determination of BEN in its insecticidal formulations and water samples, by using three different solid-phase reactors containing bulk PbO2 (B-SPR), PbO2 nanoparticles (N-SPR) and grafted nanoparticles of SiO2-PbO2 (G-SPR) immobilized on cellulose acetate matrix (CA). This method of oxidative coupling is based on alkaline hydrolysis of the BEN pesticide, and then coupled with N,N dimethyl-p-phenylenediamine sulphate (DMPD) to give a blue color product which measured at λmax 675 nm. It worth to mentioned that under optimal conditions, Beer’s law is obeyed in the range of 1-175 μg mL-1 for B-SPR and 0.25-70 μg mL-1 of BEN for both N-SPR and G-SPR respectively within limit of detection (LOD) of 0.931, 0.234 and 0.210 μg mL-1 for B-SPR N-SPR and G-SPR respectively. The surface methodology of the solid phase was also investigated by using atomic force microscopy.

Flow-Through Fourier Transform Infrared Sensor for Total Hydrocarbons Determination in Water

2009 ◽  
Vol 63 (9) ◽  
pp. 1015-1021 ◽  
Author(s):  
David Pérez-Palacios ◽  
Sergio Armenta ◽  
Bernhard Lendl
Keyword(s):  
Fourier Transform ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Chlorinated Solvents ◽  
Analytical Signal ◽  
Fourier Transform Infrared ◽  
Minimal Sample ◽  
Relative Standard ◽  
Ft Ir ◽  
Flow Through

A new flow-through Fourier transform infrared (FT-IR) sensor for oil in water analysis based on solid-phase spectroscopy on octadecyl (C18) silica particles has been developed. The C18 non-polar sorbent is placed inside the sensor and is able to retain hydrocarbons from water samples. The system does not require the use of chlorinated solvents, reducing the environmental impact, and the minimal sample handling stages serve to ensure sample integrity whilst reducing exposure of the analyst to any toxic hydrocarbons present within the samples. Fourier transform infrared (FT-IR) spectra were recorded by co-adding 32 scans at a resolution of 4 cm−1 and the band located at 1462 cm−1 due to the CH2 bending was integrated from 1475 to 1450 cm−1 using a baseline correction established between 1485 and 1440 cm−1 using the areas as analytical signal. The technique, which provides a limit of detection (LOD) of 22 mg L−1 and a precision expressed as relative standard deviation (RSD) lower than 5%, is considerably rapid and allows for a high level of automation.

scholarly journals Determination of Sodium Cromoglycate by a New Kinetic Spectrophotometric Method in Biological Samples

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Mohsen Keyvanfard ◽  
Khadijeh Alizad ◽  
Razieh Shakeri
Keyword(s):  
Standard Deviation ◽  
Sodium Cromoglycate ◽  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Micellar Medium ◽  
Relative Standard ◽  
Kinetic Spectrophotometric

A new kinetic spectrophotometric method is described for the determination of ultratrace amounts of sodium cromoglycate (SCG). The method based on catalytic action of SCG on the oxidation of amaranth with periodate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of the amaranth at 518 nm, for the first 4 min from initiation of the reaction. Calibration curve was linear in the range of 4.0−36.0 ng mL−1SCG. The limit of detection is 2.7 ng mL−1SCG. The relative standard deviation (RSD) for ten replicate analyses of 12, 20, and 28 ng mL−1SCG was 0.40%, 0.32%, and 0.53%, respectively. The proposed method was used for the determination of SCG in biological samples.

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.

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