Low volume microwave digestion and direct determination of selenium in biological samples by hydride generation-atomic fluorescence spectrometry

2010 ◽  
Vol 665 (2) ◽  
pp. 123-128 ◽  
Author(s):  
Qiu-Xiang Zhao ◽  
Yu-Wei Chen ◽  
Nelson Belzile ◽  
Mohui Wang
2012 ◽  
Vol 549 ◽  
pp. 188-192 ◽  
Author(s):  
Shu Ying Guo ◽  
Zheng Jia Ji ◽  
Bo Feng ◽  
Jiang Bian

A robust, accurate and sensitive analytical procedure was developed for the simultaneous determination of trace Antimony and Bismuth in Jilin ginseng by hydride generation atomic fluorescence spectrometry. The parameters were studied systematically, such as acid concentration of the reaction medium, flow rate of the carrier gas and shield gas, the atomizer of height, etc. Ascorbic acid and thiourea were used as reducer or masking agents to enhance the generation efficiency of the volatile species of Sb and Bi. In the presence of thiourea and ascorbic acid, the influences of some coexisting elements on the determination of antimony and bismuth were investigated.


Author(s):  
Chandrasekaran Krishnan ◽  
Venkata Balarama Krishna Mullapudi ◽  
Nidhi Garg

A single-step microwave assisted digestion (MWAD) procedure employing very dilute solutions of HNO3 was developed for the quantitative determination of bismuth in bismuth-containing pharmaceuticals by hydride generation-atomic fluorescence spectrometry (HG-AFS). Experimental parameters affecting MWAD process such as acid concentration (HNO3), digestion time and temperature were optimized to get quantitative recovery of bismuth. The studies indicated that the method is rapid (within 15 min) including cooling time and recovery > 98% was obtained using 10mL of 5% (v/v) HNO3 as digestion medium with ~0.1g of sample. The optimum microwave digestion parameters obtained were: temperature – 180oC, pressure – 25 bar and hold time - 10 min. A clear solution with negligible residue was obtained after microwave digestion. The digested sample solution was appropriately diluted with 2% (v/v) HCl for subsequent analysis by HG-AFS. The reproducibility, expressed as % RSD was lower than 2% for the allopathic medicine. Under optimal conditions, the limit of detection (LOD) for Bi was calculated to be 0.024mg/kg. The methodology was optimized using a bismuth-containing pharmaceutical – Pylobis, purchased from a local pharmacy. The optimized MWAD approach was further applied to few other bismuth-containing pharmaceutical products. The developed method has significant advantages when compared to the conventional hot-plate digestion methods reported for Bi-containing pharmaceuticals, employing large volumes of concentrated acids. These investigations revealed that the proposed MWAD method in combination with HG-AFS can be utilized for the rapid determination of Bi in pharmaceutical products on regular basis.


2014 ◽  
Vol 484-485 ◽  
pp. 62-65
Author(s):  
Xiu Jing Zhang

0.2000g mogroside sample is digested by 7.0ml nitric acid and 3.0ml hydrogen peroxide, and generated by coprecipitation enrichment hydride - atomic fluorescence spectrometry determines trace selenium in it. Under optimum experiment conditions, a standard curve was produced using selenium standard solution, the linear equation is Ise=2890.6c+0.0012,compared wish the linear relaticnship is not by coprecipitation direct determination of standard series Ise=82.56c+0.0018 Selenium detection sensitivity was increased by 35.01 times,the correlation coefficient of obtained linear regression equation is 0.9996, the detection limit is 0.0012μg/L and the relative standard deviation is 0.76% (n=5). Containing 0.1808μg.g-1 Se Luo Han Shen samples. Based on mogroside sample, add a certain of standard solution to do recovery experiment, the obtained recovery rate is in 95.8%~103.6% and the result is satisfactory.


2019 ◽  
Vol 34 (3) ◽  
pp. 526-534 ◽  
Author(s):  
Meitong Liu ◽  
Tengpeng Liu ◽  
Jixin Liu ◽  
Xuefei Mao ◽  
Xing Na ◽  
...  

In this study, the slurry sampling hydride generation (SLS-HG) system was first coupled within situdielectric barrier discharge atomic fluorescence spectrometry (DBD-AFS) for arsenic analysis in biological samples based on the gas phase enrichment (GPE) principle.


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