scholarly journals DETERMINATION OF NITRAZEPAM IN PHARMACEUTICAL PREPARATIONS USING SOLID-PHASE REACTOR - REVERSE FLOW INJECTION ANALYSIS

Author(s):  
Mariam Jamal ◽  
Hind Hadi

Objective: A simple and fast reverse flow injection system including a solid-phase reactor containing PbO2 with spectrophotometric detection was suggested for the determination of nitrazepam (NIT) in pharmaceutical tablets.Methods: The method was based on oxidation of the reagent (phloroglucinol) with PbO2 immobilized in a polymeric matrix which was then coupled with reduced NIT in aqueous medium. The pink-colored product was measured at 530 nm.Results: The calibration graph was linear over the range of 50–400 μg/mL with a relative standard deviation of <2% (n=29) and a sample throughput of 48 samples per hour. The variables of the solid-phase reactor such as composition, particle size, and length of the reactor were studied. The chemical and physical parameters, which affect the reverse flow method, were also studied.Conclusion: The oxidation reactor engaged with a flow system was successfully applied for the determination of NIT with good sensitivity and precision.

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

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.


2011 ◽  
Vol 6 (No. 4) ◽  
pp. 198-204 ◽  
Author(s):  
L. Yu ◽  
M. Wu ◽  
W. Dong ◽  
J. Jin ◽  
X. Zhang

&nbsp; In order to control the pollution by anionic surfactants in seawater, a simple, accurate and sensitive reverse flow injection (rFIA) spectrophotometric method for the determination of anionic surfactants in seawater is suggested in this paper. Sodium dodecylbenzenesulfonate (LAS) was selected as the reference anionic surfactant. The method is based on the ion associate formed between LAS and Ethyl Violet. The absorbance of the complex is measured by optical detector at 585 nm. Chemical factors and rFIA variables affecting the system are also discussed. Under the optimal conditions, the linear range of this method was 25.0&ndash;400.0 &mu;g/l; the detection limit was 2.4 &mu;g/l; the relative standard deviation was 0.38%. This method is suitable for automatic and continuous analysis, and was successfully applied to determine the content of anionic surfactants in seawater.


2012 ◽  
Vol 48 (2) ◽  
pp. 325-333 ◽  
Author(s):  
Fernando Campanhã Vicentini ◽  
Willian Toito Suarez ◽  
Éder Tadeu Gomes Cavalheiro ◽  
Orlando Fatibello-Filho

A simple flow-injection analysis procedure was developed for determining captopril in pharmaceutical formulations employing a novel solid-phase reactor containing silver thiocyanate immobilized in a castor oil derivative polyurethane resin. The method was based on silver mercaptide formation between the captopril and Ag(I) in the solid-phase reactor. During such a reaction, the SCN- anion was released and reacted with Fe3+, which generated the FeSCN2+ complex that was continuously monitored at 480 nm. The analytical curve was linear in the captopril concentration range from 3.0 × 10-4 mol L-1 to 1.1 × 10-3 mol L-1 with a detection limit of 8.0 × 10-5 mol L-1. Recoveries between 97.5% and 103% and a relative standard deviation of 2% for a solution containing 6.0 × 10-4 mol L-1 captopril (n = 12) were obtained. The sample throughput was 40 h-1 and the results obtained for captopril in pharmaceutical formulations using this procedure and those obtained using a pharmacopoeia procedure were in agreement at a 95% confidence level.


2020 ◽  
Vol 17 (1(Suppl.)) ◽  
pp. 0265
Author(s):  
Sadeem Subhi Abed

            A spectrophotometric- reverse flow injection analysis (rFIA) method has been proposed for the   determination of Nitrazepam (NIT) in pure and pharmaceutical preparations. The method is based upon the coupling reaction of NIT with a new reagent O-Coumaric acid (OCA) in the presence of sodium periodate in an aqueous solution. The blue color product was measured at 632 nm. The variation (chemical and physical parameters) related with reverse flow system were estimated. The linearity was over the range 15 - 450 µg/mL of NIT with detection limits and limit of quantification of 3.425 and 11.417 µg mL-1 NIT,respectively. The sample throughput of 28 samples per hour was achieved. Suggested method was successfully applied for the determination of NIT in its dosage forms.


2001 ◽  
Vol 84 (1) ◽  
pp. 59-64 ◽  
Author(s):  
Inês P A Morais ◽  
António O S S Rangel ◽  
M Renata S Souto

Abstract A turbidimetric flow-injection system was developed for the determination of sulfate in natural and residual water samples, with no previous treatment, using spectrophotometric detection. The precipitating agent, 7.0% (w/v) barium chloride solution prepared in 0.10% (w/v) polyvinyl alcohol, was added by using the merging-zones approach. A 100 mg/L sulfate solution in 0.07M nitric acid was mixed with the sample before it entered the injection loop to improve the detection limit, provide in-line pH adjustment, and prevent the interference of some anionic species. The relative standard deviations of the results were between 1.4 and 3.0% and were in agreement with results obtained by the reference method. Samples within a linear concentration range of 10–120 mg SO42−/L can be analyzed at a rate of 40/h. The detection limit is 5 mg SO42−/L.


2012 ◽  
Vol 2012 ◽  
pp. 1-5
Author(s):  
Jiangman Liu ◽  
Huan Yang ◽  
Yun Zhang ◽  
Min Wu ◽  
Haixiang Zhao ◽  
...  

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%.


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