Study on Speciation of As, Cr, and Sb in Bottled Flavored Drinking Water Samples Using Advanced Analytical Techniques IEC/SEC-HPLC/ICP-DRC-MS and ESI-MS/MS

Abstract

The main aim of the research was to develop a complementary analytical approach consisting of bespoke speciation analysis and non-targeted speciation analysis of As, Sb, and Cr in flavored bottled drinking water samples using HPLC/ICP-DRC-MS and ESI-MS/MS. The scope of two previously developed analytical procedures, (1) multielemental speciation procedure for As^III, As^V, Cr^VI, Sb^III, and Sb^V analysis and (2) arsenic speciation procedure for AsB, As^III, DMA, MMA, and As^V quantification, was extended to the analysis of a new sample type in terms of bespoke speciation analysis. As for the non-targeted speciation, analysis size exclusion chromatography was used with ICP-MS and a complementary technique, ESI-MS/MS, was used for the organic species of As, Sb, and Cr screening. Full validation of procedures 1 and 2 was conducted. Procedure 1 and 2 were characterized with precision values in the range from 2.5% to 5.5% and from 3.6% to 7.2%, respectively. Obtained recoveries ranged from 97% to 106% and from 99% to 106% for procedures 1 and 2, respectively. Expanded uncertainties calculated for procedures 1 and 2 ranged from 6.1% to 9.4% and from 7.4% to 9.9%, respectively. The applicability of the proposed procedures was tested on bottled drinking water samples. Results for the real samples in procedure 1 were in the range from 0.286 ± 0.027 [μg L^-1] to 0.414 ± 0.039 [μg L^-1] for As^III, from 0.900 ± 0.083 [μg L^-1] to 3.26 ± 0.30 [μg L^-1] for As^V, and from 0.201 ± 0.012 [μg L^-1] to 0.524 ± 0.032 [μg L^-1] for Sb^V. Cr^VI and Sb^III were not detected in any sample. As for procedure 2, results were in the range from 0.0541 ± 0.0053 [μg L^-1] to 0.554 ± 0.054 [μg L^-1] for AsB. Results for As^III and As^V obtained with procedure 2 were in good accordance with results obtained with procedure 1. DMA and MMA were not detected in any sample.

Keywords: bottled flavored drinking water samples; electrospray ionization mass spectrometry; high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry; method validation; speciation analysis.