Microwave-induced combustion of graphene for further determination of elemental impurities using ICP-OES and TXRF

2018 ◽  
Vol 33 (11) ◽  
pp. 1910-1916 ◽  
Author(s):  
Airui Zhang ◽  
Hai Wang ◽  
Pengfei Zha ◽  
Meiling Wang ◽  
Haifeng Wang ◽  
...  

An analytical method of microwave induced combustion (MIC) combined with ICP-OES and TXRF is proposed to determine elemental impurities in graphene.

2021 ◽  
Vol 40 (1) ◽  
pp. 35
Author(s):  
Katerina Jancevska ◽  
Gjorgji Petrushevski ◽  
Mirjana Bogdanoska ◽  
Trajce Stafilov ◽  
Sonja Ugarkovic

Fast and simple closed-vessel microwave-assisted digestion procedure was developed for decomposition of three pharmaceutical dosage forms of ibuprofen such as tablets, suspension and gel, prior to elemental impurity analysis by one robust and precise ICP-OES method. Samples were digested by four-step microwave program consisting of a 10 min temperature gradient to 180°C, maintained at 180°C for 10 min, followed by 5 min ramping time to 210°C with holding time of 10 min on 210°C. Subsequently, ICP-OES method was developed and validated for simultaneous determination of selected elemental impurities. Results of recovery studies range between 77% and 105% for each element in all analyzed formulations. Correlation coefficients of the regression equations were higher than 0.999 for all analyzed elements. Validation results reveal that the proposed method is specific, accurate, and precise and could be applied for simultaneous quantitative analysis of multi element solutions in different pharmaceutical dosage forms of ibuprofen.


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

2016 ◽  
Vol 99 (6) ◽  
pp. 1572-1575 ◽  
Author(s):  
Dayara Virgínia L Ávila ◽  
Sidnei O Souza ◽  
Silvânio Silvério L Costa ◽  
Rennan Geovanny O Araujo ◽  
Carlos Alexandre B Garcia ◽  
...  

Abstract This work describes an analytical method for Zn determination in dry feeds for cats and dogs by energy-dispersive X-ray fluorescence (EDXRF). Samples of dry feed were powdered and prepared in the form of pellets for direct analysis by EDXRF. The LOQ (10σ) was 0.4 mg/kg. The samples were also analyzed by inductively coupled plasma-optical emission spectrometry (ICP-OES) as an independent comparative method. Application of a paired t-test showed no significant differences between Zn concentrations obtained by EDXRF and ICP-OES (at a 95% confidence level). Analysis of variance was also applied to the results and revealed no significant differences between the two techniques (at a 95% confidence level). The precision, expressed as the RSD (n = 3), was RSD < 4.55%. This analytical method provides a simple, rapid, accurate, and precise determination of Zn in dry feeds for cats and dogs by EDXRF as direct, solid-sample analysis.


2020 ◽  
Vol 16 (4) ◽  
pp. 392-403
Author(s):  
Lakshmi Narasimha Rao Katakam ◽  
Hassan Y. Aboul-Enein

: Inductively coupled plasma is a new technique employed for the determination of elemental impurities in pharmaceutical ingredients viz. raw materials, drug substance, and drug product dosage forms. New US FDA and EMA regulations came into effect from Jan 2018 as industry standard requirements for the determination of inorganic elemental impurities using ICP-OES/AES or ICP-MS analytical techniques. The method development was optimized for the determination of the listed elements as per USP <232> <233> elemental impurities-limits and procedures. It also demonstrates the validation of the method and verification/transfer of the method which also provides an insight into the presence of free elemental atomics of the gaseous form of the sample (drug substance, drug product or excipients), thus helping in determining the concentration of the element of interest. Also, the regulatory guidance is very general and does not explain the sample specifications for the individual element concentrations. Thus, this review emphasizes the routine instrumental maintenance, analytical method development challenges, trends in the performance of analytical method validation and verification/ transfer activities of the various pharmaceutical dosage forms outlined with acceptance criterion.


Author(s):  
Vikas Kumar Singh ◽  
Santosh Kumar Verma ◽  
Sudhanshu Ranjan Swain

A highly selective, specific, precise sensitive and reliable ICPMS method has been developed and validated by using ICP-MS for the determination of multielement in Sucroferric oxyhydroxide. The described ICP-MS method provides specific detection and quantification of minor and trace elements from 0.3J(30%) to 2J(200%) of its individual specification of each element i.e Ag, As, Au, Ba, Cd, Co, Cr, Cu, Hg, Ir, Li, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru, Sb, Se, Sn, Tl,  and V.The analytical method found to be Linear for each individual element with working concentration range from 30%, 50%, 100%, 150% and 200% i.e 0.3J, 0.5J, 1J, 1.5J and 2J with correlation coefficient not less than 0.990.The % recoveries of elemental impurities of each individual elements at three different concentrations with spiking in samples were found to be an acceptable range as 70% to 150%.The method was found to be precise and robust and its relative standard deviation was below 20%.The actual observed relative standard deviation in Precision was found to be in an acceptable range. Therefore developed method can be use for routine quantitative analysis of elemental impurities like Ag, As, Au, Ba, Cd, Co, Cr, Cu, Hg, Ir, Li, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru, Sb, Se, Sn, Tl, and V to ensure the quality of drug product.


Author(s):  
Samir Santos ◽  
Silvânio Costa ◽  
Sidnei Souza ◽  
Karina Garcia ◽  
Sarah Soares ◽  
...  

An analytical method for multi-elementary determination in powder refreshment, based on sample digestion using dilute mineral acids and detection by inductively plasma coupled optical emission spectrometry (ICP OES) is proposed. Chemometric tools, such as fractional factorial design and principal component analysis (PCA) and hierarchical cluster analysis (HCA) were applied to optimize the sample preparation conditions in closed block digester, and Doehlert design for spectrometer operation. Addition and recovery tests and analyses of certified reference material were performed to evaluate the precision and accuracy, and the results confirm the reliability of the proposed method. Limits of quantification (LOQ) between 0.02 and 36 μg g−1 were obtained. The analytical method was applied for determination of 24 inorganic constituents in 20 powder refreshment samples. Calcium, K, Mg, Na, P, S and Ti presented the highest concentrations. The analytical method was adequate for the determinations of inorganic constituents in powder refreshment samples by ICP OES.


2020 ◽  
Vol 0 (4) ◽  
pp. 29-32
Author(s):  
B.M. GAREEV ◽  
◽  
A.M. ABDRAKHMANOV ◽  
G.L. SHARIPOV ◽  
◽  
...  

The photoluminescence of carbon quantum dots synthesized from natural honey and mixtures of honey and sugar has been studied. An increase in the sugar content leads to a decrease in the photoluminescence intensity without changing the shape of the luminescence spectrum of these quantum dots aqueous solutions, which is associated with a decrease in the yield of their synthesis in the sugar presence. The discovered effect can be used to detect sugar in honey. When examining five different market samples of flower honey using this method, two of them showed a significant decrease in the photoluminescence intensity. A laboratory test for compliance with GOST 19792-2017 Standard requirements established an excess of the sucrose content in these samples. Luminescent determination of sugar in honey does not require complicated equipment and can be used to develop a new analytical method for determining the sugar content in counterfeit natural honey.


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