scholarly journals Determinação de rutina em formulações farmacêuticas utilizando um sistema de análise por injeção em fluxo envolvendo multicomutação

2017 ◽  
Vol 41 (1) ◽  
pp. 32
Author(s):  
Déborah C. Azzi ◽  
Geiser G. Oliveira ◽  
Bruno C. Janegitz ◽  
Viviane G. Bonifácio ◽  
Orlando Fatibello-Filho ◽  
...  

This paper reports a flow injection chemiluminescence method involving multicommutation for rutin determination in pharmaceutical formulations. The method is based on the oxidation of rutin by sodium hypochlorite which decreases the signal magnitude when compared with the same reaction without the rutin. Under optimized conditions, an analytical curve was obtained for rutin concentration range from 5.0 × 10-6 mol L-1 to 1.0 × 10-4 mol L-1 (r = 0.9966) with detection limit of 9.7 × 10-7 mol L-1 and a sampling frequency of 120 h-1. Repeatability study for a 7.0 × 10-6 mol L-1 rutine concentration showed a relative standard deviation (RSD) less than 5.0% for ten consecutives determination. The proposed method was applied successfully for rutin determination in pharmaceutical products.

2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.


2008 ◽  
Vol 33 (2) ◽  
pp. 47-54 ◽  
Author(s):  
O. Fatibello-Filho ◽  
H. J. Vieira

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.


2001 ◽  
Vol 84 (4) ◽  
pp. 1011-1016 ◽  
Author(s):  
Jing-Fu Liu ◽  
Ying-Di Feng ◽  
Gui-Bin Jiang

Abstract A simple and rapid flow injection spectrophotometric procedure was developed for determination of manganese. In the presence of pyrophosphate and acetate, manganese was immediately oxidized to permanganate by periodate at room temperature in slightly alkaline medium. Under optimized conditions, the determination was made with a sampling rate of 120/h, a linear range of 0–30 mg/L Mn(II), a detection limit (S/N = 3) of 0.08 mg/L, and a relative standard deviation of 0.6% (n = 11) at 10 mg/L Mn(II). The proposed method was used to determine manganese in trace mineral premixes and feedstuffs. Results agreed well with those obtained by the standard atomic absorption spectroscopy method.


2011 ◽  
Vol 26 (6) ◽  
pp. 349-355 ◽  
Author(s):  
Hairu Lv ◽  
Xijuan Tan ◽  
Yun Zhang ◽  
Zhenghua Song

An ultrasensitive method for determining picomolar midecamycin (MID) by flow injection (FI) chemiluminescence (CL) was first described based on the inhibitory effect of MID on luminol–BSA reaction. It was found that the CL intensity decrements were linear with the logarithm of MID concentrations in the range of 1.0–5000 pmol · l–1with a detection limit as low as 0.3 pmol · l–1(3σ). The relative standard deviation of seven repetitive measurements for 10 pmol · l–1MID was 3.0%. At a flow rate of 2.0 ml · min–1, the whole analysis procedure including sampling and washing could be finished in 30 s, offering the sample efficiency of 120 h–1. This proposed method was successfully applied to determine MID in human serum samples with the recoveries from 96.0 to 110.0%. The CL mechanism of luminol–BSA–MID reaction was also given.


2007 ◽  
Vol 21 (2) ◽  
pp. 135-141 ◽  
Author(s):  
Xiaofei Gao ◽  
Houyong Liu ◽  
Zhenghua Song ◽  
Xili He ◽  
Faxin Dong

A novel chemiluminescence method for the assay of sudan I was designed using flow injection with chemiluminescence detection. The proposed method was based on the increment effect of sudan I on the chemiluminescence intensity in the luminol–KIO4system. The increment of chemiluminescence intensity was correlated with the sudan I concentration in the range from 0.1 to 10 pg ml−1, and the determination could be performed in 0.5 min in flow rate of 2 ml min−1, including sampling and washing, giving a throughput of 120 h−1with a relative standard deviation of less than 5.0%. The method had been successfully applied to the assay of sudan I in Pixian douban, Golden mark guilin chilli sauce and Golden mark satay sauce, and the recovery was 90.0–103.8%.


2009 ◽  
Vol 15 (2) ◽  
pp. 69-76 ◽  
Author(s):  
S.M. Al-Ghannam ◽  
A.M. Al-Olyan

A sensitive spectrophotometric method was developed for the determination of some 1,4-dihydropyridine compounds namely, nicardipine and isradipine either in pure form or in pharmaceutical preparations. The method is based on the reduction of nicardipine and isradipine with zinc powder and calcium chloride followed by further reduction with sodium pentacyanoaminoferrate (II) to give violet and red products having the absorbance maximum at 546 and 539 nm with nicardipine and isradipine, respectively. Beer's law was obeyed over the concentration range 8.0-180 ?g/ml with the detection limit of 1.67 ?g/ml for nicardipine and 8.0-110 ?g/ml with the detection limit of 1.748 ?g/ml for isradipine. The analytical parameters and their effects on the reported methods were investigated. The molar absorptivity, quantization limit, standard deviation of intercept (Sa), standard deviation of slope (Sb) and standard deviation of the residuals (Sy/x) were calculated. The composition of the result compounds were found 1:1 for nicardipine and 1:2 for isradipine by Job's method and the conditional stability constant (Kf) and the free energy changes (?G) were calculated for compounds formed. The proposed method was applied successfully for the determination of nicardipine and isradipine in their dosage forms. The results obtained were in good agreement with those obtained using the reference or official methods. A proposal of the reaction pathway was presented.


2013 ◽  
Vol 10 (3) ◽  
pp. 1005-1013 ◽  
Author(s):  
Baghdad Science Journal

A simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations (tablets) and industrial wastewater samples. The proposed method was validated by sensitivity and precision which proves suitability for the routine analysis of tadalafil in true samples.


2012 ◽  
Vol 535-537 ◽  
pp. 1337-1340 ◽  
Author(s):  
Chi Yang ◽  
Nai Lin Ren

A new chemiluminescence system was built by using gadolinium as sensitizer, and the analysis capabilities of this system was tested as below. The method is based on chemluminescence of Ce (IV)-SO32- sensitized by Gd3+-OFLX. The effects of some critical experimental conditions were discussed and the optimum conditions for chemluminescence emission were investigated. The linear relationship between the relative chemiluminescence intensity and the concentration of OFLX is in the range of 2×10-9 g/mL~5×10-7 g/mL with a detection limit of 1.0×10-9g/mL .The relative standard deviation is 2.8% (n=11) for a level of 5.0×10-7 g/mL. The method has been applied to the analysis of OFLX in tablets with satisfactory results.


2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Muhammad Asgher ◽  
Mohammad Yaqoob ◽  
Abdul Nabi ◽  
Ghulam Murtaza ◽  
Abdul Rauf Siddiqi ◽  
...  

Rose Bengal photosensitized flow injection chemiluminescence method is reported using luminol-Cu(II) for the determination of vitamins A and C in pharmaceutical formulations. The reaction is based on the enhancement effect of analyte in the production of anion radicals of Rose Bengal (RB•−) which rapidly interact with dissolved oxygen and generate superoxide anions radicals (O2•−) and hydrogen peroxide (H2O2). Highly reactive hydroxyl radicals (•OH) were produced via dismutation of H2O2by catalyst (Cu2+). The generated superoxide anions radicals and hydroxyl radicals thus oxidize luminol in alkaline medium to generate strong chemiluminescence. The limit of detection (3sof the blank,n=6) of vitamins A and C and RB was found to be 0.008, 0.005, and 0.05 μg mL−1, respectively. The sample throughput of 70 h−1for vitamins A and C and 30 h−1for RB was found. Calibration curve was linear in the range of 0.05–15, 0.01–20, and 0.1–50 μg mL−1for vitamins A and C and RB, respectively, with relative standard deviations (RSDs;n=3) in the range 1.6–3.6%. The method was successfully applied to pharmaceutical formulations and the results obtained were in good agreement with the labeled values.


2013 ◽  
Vol 699 ◽  
pp. 34-39
Author(s):  
Li Liu ◽  
Xia Shi Zhu

A new Triton X-114 cloud point extraction combined with fluorometry method for analysis of magnolol in drug samples was developed. Under the optimum conditions, the calibration graph was linear in the range of 2.0-150.0ng/mL of magnolol in the initial solution with r = 0.9998. Detection limit (DL) was 0.03ng/mL (S/N=3) and the relative standard deviation (RSD) for 20.0ng/mL of magnolol was 2.79%(n=11). The method was successfully applied for the determination of magnolol in drug samples with satisfactory results.


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