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

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 INJECTION SPECTROPHOTOMETRIC DETERMINATION OF NARINGENIN IN SUPPLEMENTS USING SOLID-PHASE REACTOR CONTAINING IMMOBILIZED MANGANESE DIOXIDE

Objective: Naringenin (NAR) is a part of the human daily diet, and it plays an important role in human health for its biological functions. This study describes a new, sensitive, simple, and accurate method for determining NAR in supplements.Methods: The method is based on oxidative coupling reaction between NAR and N, N-dimethyl-p-phenylenediamine in an alkaline medium using manganese dioxide immobilized in cellulose acetate as online oxidant agent to form a colored product which can be monitored at λ max598 nm. Results: Several operating parameters such as reactor column length, particles size, chemicals, and physicals reaction conditions were studied. The proposed method was sensitive and good repeatable, the linear range of NAR concentration was from 1 to 70 μg/ml with a limit of detection of 0.292 μg/ml, and recovery range of analysis was 99.55–100.48%. Conclusion: The proposed method was successfully applied for determining NAR in supplements.

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

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.

A low-cost automated flow analyzer based on low temperature co-fired ceramic and LED photometer for ascorbic acid determination

An automated flow analyzer based on low temperature co-fired ceramic (LTCC), a solid-phase reactor (SPR) and a low-cost photometer was designed for ascorbic acid (AA) determination in pharmaceutical formulations. It consists of a peristaltic pump, three-way solenoid valves, SPR to chemically convert Cu(II) into Cu(I), and a LTCC device for mixing the liberated copper with bathocuproine and detection. The flow cell in the LTCC employed an ultrabright LED — photodiode photometer. The analyzer successfully determined AA in pharmaceutical formulations. The analytical curve from 8.5×10−6 to 7.0×10−4 M gave a detection limit of 7.0×10−7 M and a RSD of 2.1% for a 2.0×10−4 M AA solution (n = 10). A high sampling frequency of 102 h−1 and low reagent and sample consumption (150 µL) resulted.

Flow-injection spectrophotometric determination of dipyrone in pharmaceutical formulations using a solid-phase reactor with copper(II) phosphate

In this work, a flow-injection spectrophotometric method for dipyrone determination in pharmaceutical formulations was developed. Dipyrone sample solutions were injected into a carrier stream of deionized water and the reaction was carried out in a solid-phase reactor (12 cm, 2.0 mm i.d.) packed with Cu3(PO4)2(s) entrapped in a matrix of polyester resin. The Cu(II) ions were released from the solid phase reactor by the formation of Cu(II)-(dipyrone)n complex. When the complex is released, it reacts with 0.02% m/v alizarin red S in deionized water to produce a Cu(VABO3)3 complex whose absorbance was monitored at 540 nm. The calibration graph was linear over the range 5.0×10−5–4.0×10−4 mol L−1 with a detection limit of 2.0×10−5 mol L−1 and relative standard deviation for 10 successive determinations of 1.5% (2.0×10−4 mol L−1 dipyrone solution). The calculated sample throughput was 60 h−1. The column was stable for at least 8 h of continuous use (500 injections) at 25°C. Pharmaceutical formulations were analyzed and the results from an official procedure measurement were compared with those from the proposed FIA method in order to validate the latter method.