Decomposition of six common selenium species found in animal tissues using microwave digestion with nitric acid and ICP-MS

2016 ◽  
Vol 126 ◽  
pp. 92-95 ◽  
Author(s):  
W. Maher ◽  
F. Krikowa ◽  
S. Foster
Author(s):  
Sameer Amereih ◽  
Thomas Meisel ◽  
Wolfhard Wegsheider

Two independent digestion techniques (microwave acid digestion with HF and HCl, HNO3 and Na2O2 sintering, respectively) were applied to determine the total Sb concentration in a real soil sample and in reference materials: Icelandic Basalt (BIR-1), Cody Shale (SCo-1) and (Soil-7). ICP-MS was used to determine total antimony concentrations in the digested and the extracted solutions using external calibration and isotope dilution technique. The recoveries of Sb using HF in the acids digestion mixture in closed-vessels microwave digestion system were excellent and the concentrations are in very good agreement with certified or reported concentrations of reference materials. Using closed-vessels combined with microwave heating systems probably prevents the loss of volatile Sb compounds. The use of hydrogen fluoride with other strong acid can help dissociating insoluble antimony silicates. Different extraction reagents were tested for their ability to extract antimony using an ultrasonic bath namely: EDTA disodium salt, potassium hydroxide, citric acid monohydrate, pyridine-2,6-dicarboxylic acid, ammonium acetate, ammonium oxalate, ammonium thiocyanate, ammonium persulphate and di-ammonium hydrogen citrate. A 500 mmol L-1 solution of citric acid pH 1.08 proved to be the most efficient extractant. Optimization of the extraction conditions were investigated by studying the effect of pH, concentration, temperature, time of extraction, the ratio of sample mass to the volume of extractant and the number of consecutive extractions. As a result three consecutive extractions for a total time of 45 min at 80 ˚C was the most efficient condition for Sb extraction. Using these extraction conditions 61%, 3.7% RSD and 42%, 2.2% RSD (n=6) of the total antimony in the real soil and Soil-7 samples, respectively could be extracted.


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.


1989 ◽  
Vol 35 (3) ◽  
pp. 488-490 ◽  
Author(s):  
J R Nicholson ◽  
M G Savory ◽  
J Savory ◽  
M R Wills

Abstract We describe a simple and convenient method for processing small amounts of tissue samples for trace-metal measurements by atomic absorption spectrometry, by use of a modified Parr microwave digestion bomb. Digestion proceeds rapidly (less than or equal to 90 s) in a sealed Teflon-lined vessel that eliminates contamination or loss from volatilization. Small quantities of tissue (5-100 mg dry weight) are digested in high-purity nitric acid, yielding concentrations of analyte that can be measured directly without further sample manipulation. We analyzed National Institute of Standards and Technology bovine liver Standard Reference Material to verify the accuracy of the technique. We assessed the applicability of the technique to analysis for aluminum in bone by comparison with a dry ashing procedure.


2014 ◽  
Vol 32 (No. 4) ◽  
pp. 354-359 ◽  
Author(s):  
M. Jarošová ◽  
D. Milde ◽  
M. Kuba

We determined the mineral nutrients and toxic elements (Ca, Cu, Fe, Mg, Zn, Cd, Cr, Mn, Ni, and Pb) in five types of coffee by atomic absorption spectrometry and inductively coupled plasma mass spectrometry. The decomposition of the samples took place in a microwave digestion system with HNO<sub>3</sub> and H<sub>2</sub>O<sub>2</sub> reagents. Partial validation of the method was performed by using the certified reference material (NCS ZC 73014). Univariate and multivariate statistical methods were used to compare both the coffee samples and the techniques used. No significant differences were found between two used methods. Significant differences occurred between the coffee samples but only the application of multivariate statistics helps to distinguish among samples from different locations.


2002 ◽  
Vol 50 (20) ◽  
pp. 5722-5728 ◽  
Author(s):  
Anne P. Vonderheide ◽  
Kazimierz Wrobel ◽  
Sasi S. Kannamkumarath ◽  
Clayton B'Hymer ◽  
Maria Montes-Bayón ◽  
...  
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