scholarly journals Determination and uncertainty analysis of inorganic arsenic in rice by UHPLC-ICPMS

2021 ◽  
Vol 64 (2) ◽  
pp. 251-259
Author(s):  
Rajesh Rangasamy ◽  
Praveen Kumar Malekadi ◽  
D. Peer Mohamed ◽  
Dheeraj Kumar Tyagi ◽  
Rahul Raveendran ◽  
...  

The present study arose from the need of to determine inorganic arsenic (iAs) at low levels in rice. Ultra-high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (UHPLC-ICPMS) using Kinetic Energy Discrimination (KED) mode to eliminate spectral interferences was used for analysis of iAs. Sample preparation involves extraction of inorganic arsenic (sum of As3+ and As5+) with water by heating at 90 °C for 5 min in water bath. Separation is accomplished with a reversed-phase ion pack column using a gradient chromatographic method followed by ICPMS analysis within 5 min. The method was validated in accordance with Commission Regulation (EU) No 836/2011 and performance characteristics were verified. Acceptable values were obtained for specificity, repeatability (HorRatr < 0.6), within-lab reproducibility (HorRatR < 0.3) with recovery 80-90%, limit of quantification (0.02 mg/kg), fitness-for-purpose and trueness (using CRM); thus, the method can be considered for official control purposes.

2005 ◽  
Vol 277-279 ◽  
pp. 431-437 ◽  
Author(s):  
Kyung Su Park ◽  
Jeong Sook Kim ◽  
Hyo Min Lee ◽  
Hee Soo Pyo ◽  
Soon Tae Kim ◽  
...  

Extracts of 33 samples of seaweed, shrimp, fish and shellfish, including two certified reference materials, were investigated for their contents of arsenic compounds (arsenic speciation).An anion exchange high performance liquid chromatography procedure was optimized to separate six arsenic compounds present in the seafood samples with dynamic reaction gas cell by inductively coupled plasma mass spectrometry. The concentration of each species in the sample were: arsenobetaines - 0.019-1.04 mg/kg, arsenocholine - 0.033-69.0 mg/kg, arseniousacid - ND-1.25 mg/kg, dimethylarsinate - ND-3.75 mg/kg, monomethylarsonate - ND-8.33 mg/kg, arsenic acid - ND-0.55 mg/kg. Additionally, unknown arsenic species were present in most of samples. The intake of inorganic arsenic via ingestion of the seafood samples that were analyzed did not represent a toxicological problem to humans. The limits of detection (LOD) were in the range of 0.5-2.5 µg/kg .


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