Flow injection spectrofluorimetric determination of iron(III) in water using salicylic acid

2010 ◽  
Vol 64 (4) ◽  
Author(s):  
Adem Asan ◽  
Muberra Andac ◽  
Ibrahim Isildak
Keyword(s):  
Salicylic Acid ◽  
Flow Injection ◽  
Limit Of Detection ◽  
Sampling Rate ◽  
Linear Calibration ◽  
Fluorimetric Determination ◽  
Buffer Solution ◽  
Quenching Effect ◽  
Relative Standard

AbstractA simple and fast flow injection fluorescence quenching method for the determination of iron in water has been developed. Fluorimetric determination is based on the measurement of the quenching effect of iron on salicylic acid fluorescence. An emission peak of salicylic acid in aqueous solution occurs at 409 nm with excitation at 299 nm. The carrier solution used was 2 × 10−6 mol L−1 salicylic acid in 0.1 mol L−1 NH4+/NH3 buffer solution at pH 8.5. Linear calibration was obtained for 5–100 μg L−1 iron(III) and the relative standard deviation was 1.25 % (n = 5) for a 20 μL injection volume iron(III). The limit of detection was 0.3 μg L−1 and the sampling rate was 60 h−1. The effect of interferences from various metals and anions commonly present in water was also studied. The method was successfully applied to the determination of low levels of iron in real samples (river, sea, and spring waters).

Rapid Determination of Sulfite by Flow Injection Analysis Based on Fuchsin′s Addition

2013 ◽  
Vol 295-298 ◽  
pp. 950-953 ◽  
Author(s):  
Dong Yuan ◽  
Da You Fu ◽  
Wen Yuan Tan
Keyword(s):  
Flow Injection ◽  
Addition Reaction ◽  
Rapid Determination ◽  
Sampling Rate ◽  
Optimum Conditions ◽  
Linear Calibration ◽  
Relative Standard ◽  
Replicate Measurements ◽  
Good Agreement

A rapid spectrophotometric method for flow injection determination of sulfite in tan wastewater is described. The proposed method was based on the addition reaction of sulfite with fuchsin in Na2B4O7-NaOH medium. The optimum conditions allow a linear calibration range of 0.01-1.20 μg ml-1 SO32-. The detection limit is 0.0023μg ml-1 (S/N=3), and the relative standard deviation for night replicate measurements is 1.1% for 0.5μg ml-1 of sulfite. The sampling rate is 60 samples h-1. The procedure has been applied to the determination of sulfite in tan wastewater. The results were in good agreement with those obtained by pararosaniline method.

scholarly journals Spectrophotometric flow injection system for determination of Zn2+ in ophthalmic formulations using Alizarin red S

2018 ◽  
Vol 34 (2) ◽  
pp. 67
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira
Keyword(s):  
Flow Injection ◽  
Sampling Rate ◽  
Alizarin Red S ◽  
Injection System ◽  
Borate Buffer Solution ◽  
Buffer Solution ◽  
Solution Ph ◽  
Alizarin Red ◽  
Relative Standard

A spectrophotometric flow injection method for the determination of Zn(II) in ophthalmic formulations was developed. In this work, Zn(II) ion was complexed with Alizarin red S in borate buffer solution (pH 9.0) and the chromophore produced was monitored at 520 nm. The analytical curve was linear in the Zn(II) concentration range from 6.05 x 10-6 to 1.50 x 10-4 mol L-1 with a detection limit of 3.60 x 10-6 mol L-1. Recoveries ranged from 96.3 to 105 % and a relative standard deviation of 1.2 % (n = 10) for 5.5x10-5 mol L-1 Zn(II) reference solution were obtained. The sampling rate was 60 h-1 and the results obtained of Zn(II) in ophthalmic products using this procedure are in close agreement with those obtained using a comparative spectrophotometric procedure at 95 % confidence level.

scholarly journals Spectrophotometric flow injection system for determination of Zn2+ in ophthalmic formulations using Alizarin red S

2009 ◽  
Vol 34 (2) ◽  
pp. 67-72 ◽  
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira
Keyword(s):  
Flow Injection ◽  
Sampling Rate ◽  
Alizarin Red S ◽  
Injection System ◽  
Borate Buffer Solution ◽  
Buffer Solution ◽  
Solution Ph ◽  
Alizarin Red ◽  
Relative Standard

A spectrophotometric flow injection method for the determination of Zn(II) in ophthalmic formulations was developed. In this work, Zn(II) ion was complexed with Alizarin red S in borate buffer solution (pH 9.0) and the chromophore produced was monitored at 520 nm. The analytical curve was linear in the Zn(II) concentration range from 6.05 x 10-6 to 1.50 x 10-4 mol L-1 with a detection limit of 3.60 x 10-6 mol L-1. Recoveries ranged from 96.3 to 105 % and a relative standard deviation of 1.2 % (n = 10) for 5.5x10-5 mol L-1 Zn(II) reference solution were obtained. The sampling rate was 60 h-1 and the results obtained of Zn(II) in ophthalmic products using this procedure are in close agreement with those obtained using a comparative spectrophotometric procedure at 95 % confidence level.

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 <0.46 and <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.

scholarly journals Determination of Picogram Levels of Roxithromycin in Pharmaceutical, Human Serum, and Urine by Flow-Injection Chemiluminescence

2012 ◽  
Vol 2012 ◽  
pp. 1-5
Author(s):  
Jiangman Liu ◽  
Huan Yang ◽  
Yun Zhang ◽  
Min Wu ◽  
Haixiang Zhao ◽  
...  
Keyword(s):  
Human Serum ◽  
Flow Injection ◽  
Limit Of Detection ◽  
Inhibitory Effect ◽  
Injection System ◽  
Relative Standard ◽  
Flow Injection System ◽  
Flow Injection Chemiluminescence ◽  
Serum And Urine

A sensitive chemiluminescence (CL) method, based on the inhibitory effect of roxithromycin (ROX) on the CL reaction between luminol and dissolved oxygen in a flow-injection system, was first proposed for the determination of ROX at picogram levels. The decrement of CL intensity was linearly proportional to the logarithm of ROX concentrations ranging from 0.1 to 100 pg mL-1, giving the limit of detection (LOD) of 0.03 pg mL-1 (3σ). At a flow rate of 2.0 mL min-1, a complete analytical procedure including sampling and washing could be performed within 0.5 min, with relative standard deviations (RSDs) of less than 5.0% (n=5). The proposed procedure was applied successfully to the determination of ROX in pharmaceutical, human serum, and urine with the recoveries ranging from 90.0 to 110.0%.

scholarly journals Spectrophotometric and RP-HPLC Methods for Determining Cefotaxime Sodium in Pharmaceutical Preparations

2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe
Keyword(s):  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

A rapid, simple and sensitive spectrophotometric and RP-HPLC methods have been developed for the quantitative determination of cefotaxime-Na in both pure and dosage forms. The spectrophotometric method was based on diazotization of cefotaxime-Na and then coupling with 8-hydroxyquinoline in an alkaline medium. The resulting azo dye exhibited maximum absorption at 551 nm with a molar absorptivity of 0.597 × 104 L mol-1 cm-1. Beer′s law was obeyed over the range 10-700 μg/25 mL (i.e. 0.4-28.0 ppm) with an excellent determination coefficient (R2 = 0.9993). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0194 and 0.3765 μg mL-1, respectively. The recoveries were obtained in the range 97.3-102.5% and the relative standard deviation (RSD) was better than ± 1.56. The HPLC method has been developed for the determination of cefotaxime-Na. The analysis were carried out on a C18 column and a mobile phase composed of acetonitrile and phosphate buffer solution (0.024M KH2PO4 and 0.01M H3PO4) at pH 3.5 in the ratio of 60:40 (v:v), with a flow rate of 1.0 mL min-1 and UV detection at 258 nm. The proposed method showed good linearity (in a range of concentration 1.0-200 μg mL-1. The recovery percent and a relative standard deviations were found in the range 96 to 104.8% and ± 0.017 to ± 0.031%, respectively. Both methods were applied successfully to the assay of cefotaxime-Na in commercial injection preparations.

scholarly journals A fully automated flow injection atomic absorption system for the determination of copper traces in waters with on-line pre-concentration in an ion-exchange column

1995 ◽  
Vol 17 (1) ◽  
pp. 25-29 ◽  
Author(s):  
J. L. Burguera ◽  
M. Burguera ◽  
P. Carrero ◽  
J. Marcano ◽  
C. Rivas ◽  
...  
Keyword(s):  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Flow Injection ◽  
Water Samples ◽  
Absorption Spectrometry ◽  
Linear Calibration ◽  
Relative Standard ◽  
On Line ◽  
Determination Of Copper

The paper describes the development of an automatic on-line column pre-concentration technique using a time based-flow injection atomic absorption spectrometry system. A manifold incorporating a micro-column containing 25 mg of Dowex 50W-X8 was used with a time-based injector for the pre-concentration and determination of copper in natural and drinking waters. The system features depend on the alternate positions of a solenoid valve. The 3σ detection limits, enrichment factors, sampling frequency, relative standard deviations and linear calibration graphs were, respectively, in the range 0.6-1.5 μg/l, 25-60, 15-30 measurements/h, 1.0-3.1% and 1-65 μg/ml for pre-concentration times of 1 min. The procedure was successfully applied to a range of water samples and the accuracy was assessed through recovery experiments, the analysis of certified reference water samples and by independent analysis by atomic absorption spectrometry with electrothermal atomization.

Voltammetric study of secnidazole and its determination in pharmaceutical tablet using 1, 4-benzoquinone modified carbon paste electrode

2019 ◽  
Author(s):  
Chem Int
Keyword(s):  
Carbon Paste Electrode ◽  
Limit Of Detection ◽  
Modified Carbon Paste Electrode ◽  
Carbon Paste ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Pharmaceutical Tablet ◽  
Relative Standard ◽  
Paste Electrode

In this study voltammetric behaviour of secnidazole (SCZ) at 1, 4-Benzoquinone Modified Carbon Paste Electrode (1,4-BQMCPE) was investigated in Britton Robinson buffer solution using cyclic voltammetric technique. A well-defined cathodic peak was observed for the SCZ in the entire pH range. The current increases steadily with scan rate and the results indicated that the process is irreversible reduction and adsorption controlled. The number of electrons transferred and different kinetic parameters like transfer coefficient and rate constant were calculated by using cyclic voltammetry technique. Differential pulse voltammetric method has been used for the determination of SCZ content in pharmaceutical tablet. This method enabled to determine SCZ in the concentration range 1.0 × 10-8 to 4.0 × 10-4 M. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 2.13 × 10-9 and 2.85 × 10-9 respectively. The method was applied to determine the content of SCZ in different sample solutions of SCZ tablet with excellent recovery and relative standard deviation results (99.892±1.53 respectively) for spiked standard SCZ in tablet sample solutions. The selectivity of the method for SCZ was further studied in the presence of selected potential interferents such as fluconazole, azithromycin etc and confirmed the potential applicability of the developed method for the determination of SCZ in real pharmaceutical tablets.

Determination of Trace Cobalt in Water by Reversed Flow Injection Spectrophotometry

2014 ◽  
Vol 955-959 ◽  
pp. 1276-1279
Author(s):  
Ling Su ◽  
Heng Shen Xie
Keyword(s):  
Flow Injection ◽  
Affecting Factors ◽  
Industrial Waste Water ◽  
Buffer Solution ◽  
Relative Standard ◽  
Relationship Of ◽  
The Relationship ◽  
Catalytic Effects ◽  
Coexisting Ions

A method for determination of cobalt in water by flow injection spectrophotometry based on the catalytic effects of cobalt on the oxidation reaction of arsenazo III by potassium bichromate in HAc-NaAc buffer solution of pH 4.6 was established. The relationship of the reduced absorbency to the concentration of cobalt was good linearity and the maximum absorption peak located at 550 nm. The affecting factors on the strength of absorption including acidity, dosage, temperature, coexisting ions and so on, and the optimal conditions of the reaction in the system were investigated. Calibration graphs were linear for ranges of 0 to 20 μg/mL and a detection limit of 0.3 μg/mL cobalt was achieved. The proposed method was successfully applied to the analyses of industrial waste water samples, with relative standard deviation of less than 1.5% and the recoveries are 95.1% to 96.8%for the determination of cobalt.

Flow Injection Determination of Acetylsalicylic Acid in Pharmaceutical Preparations with an Amperometric Detector

2000 ◽  
Vol 65 (6) ◽  
pp. 954-962 ◽  
Author(s):  
Jorge M. P. J. Garrido ◽  
José L. F. C. Lima ◽  
Cristina D. Matos
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Flow Injection ◽  
Sampling Rate ◽  
Hydrolysis Product ◽  
Pharmaceutical Preparations ◽  
Amperometric Detection ◽  
Automated Method ◽  
Pre Treatment

This paper reports on an automated method based on a flow injection analysis single stream system with amperometric detection for the determination of acetylsalicylic acid in pharmaceutical preparations. The amperometric detection is based on the measurement at 0.8 V vs Ag/AgCl of the current generated when the acetylsalicylic acid hydrolysis product, salicylic acid, is oxidised at a glassy carbon electrode. The current produced is directly related to the concentration of the electroactive specie and the salicylic acid content is proportional to the level of acetylsalicylic acid present in the sample, thus it is possible to determine the concentration of acetylsalicylic acid electrochemically. This system allows a sampling rate of 150 samples per hour without requiring any pre-treatment, apart from dissolving them in a NaOH/KCl buffer, pH 13.0. The results obtained were compared with those obtained using reference methods and demonstrated excellent agreement with relative deviation always lower than 2%.

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