Determination of elemental impurities of Arsenic, Cadmium, Mercury, Lead and Palladium content in Testosterone propionate by using ICP-MS

Author(s):  
Suresh P. ◽  
Konda Ravi Kumar

The aim of the present work is to develop and establish a validated analytical method for the determination of arsenic, cadmium, mercury, lead and palladium content in testosterone propionate by using inductive coupled plasma mass spectroscopy (ICP-MS). Samples were analyzed after a preparation of sample solution by dissolving in suitable solvents of concentrated nitric acid and concentrated hydrochloric acid. In the present method, RF power of 1550 watts, RF matching is 1.80 V, nebulizer flow of 0.10 rps and plasma view at spectrum mode were used. Octopole conditions are He flow is on, He flow rate is 4.3 mL/min and energy discrimination is 3.0 V were used. Significant savings in sample volumes, reagents, analysis cost and time are realized. Arsenic, cadmium, mercury, lead and palladium are primary concerned due to their high toxicity and potential contaminants should be limited in testosterone propionate and the developed method was validated according to ICH and USP guidelines. The correlation coefficient, recovery rate, LOD and LOQ reached the acceptable limits. The validated method was selective, sensitive, rapid and capable of the determination of elemental impurities of arsenic, cadmium, mercury, lead and palladium content in bulk drugs.

2020 ◽  
Vol 2 (1) ◽  
Author(s):  
Iva KOTALOVÁ ◽  
Katrin CALÁBKOVÁ ◽  
Martina NOVÁČKOVÁ ◽  
Silvie DRABINOVÁ ◽  
Silvie HEVIÁNKOVÁ

Polychlorinated substances, polyaromatic hydrocarbons, heavy metals and pesticides are among the priority even at low concentrations. The problem, however, is that such low concentrations are impossible to measure using most available methods. This researchfocused on the determination of selected priority substances – heavy metals, namely lead and cadmium, in which the determination ofPb and Cd in wastewater by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) was preceded by water sample pre-treatment.The paper deals with the influence of the pre-treatment on the resulting measured values. Two processes were selected as pre-treatmentprocesses. The first pre-treatment procedure was a simple filtration using a filter paper for moderate filtration. As the second procedure, we applied decomposition of the sample by nitric acid in the open system. The pre-treated wastewater samples were subsequentlyexamined using ICP-MS. Based on the obtained results, we can conclude that decomposition of the sample by nitric acid in the opensystem is a more suitable pre-treatment method for water samples


Talanta ◽  
2017 ◽  
Vol 171 ◽  
pp. 291-306 ◽  
Author(s):  
Inmaculada de la Calle ◽  
Mathieu Menta ◽  
Marlène Klein ◽  
Fabienne Séby

Author(s):  
Nief Rahman Ahmed ◽  
◽  
Najlaa Saadi Sheet ◽  

A new, accurate, sensitive and simple indirect spectrophotometric method for the estimation of sodium 2-mercaptoethanesulfonate (mesna) has been developed. This procedure base on the reaction of mesna with excess of silver nitrate and a known amount of methyl orange and the increase in absorbance at 520 nm, caused by a decrease in pH due to release of nitric acid, is measured and related to drug concentration .The absorbance results increased with increasing concentration of mesna . Beer’ s law is obeyed and linear at the concentration range of 2-28µg/ml. Apparent molar absorbance, Sand ell’s sensitivity values were 7.16×103 Lmol-1cm-1. And 22.93 ng.cm-2 respectively, The present method is considered to be simple because it does not need either heating or hydrolysis or solvent extraction steps. The ingredients often formulated with Metoclopramide hydrochloride have been shown not to interfere, and the proposed method is suitable for the routine determination of mesna. The (RSD) of this method was less than 2 and average recovery (accuracy) is 100 ± 0.75. The method applied successfully for estimation of mesna in (tablets and injections pharmaceutical formulations).and Application to Content Uniformity Testing


Author(s):  
Mario H. Gonzalez ◽  
Caroline S. da Silva ◽  
Clarice D. B. Amaral ◽  
Silmara R. Bianchi ◽  
Luciano H. B. de Oliveira ◽  
...  

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