Development and validation of a single run method based on species specific isotope dilution and HPLC-ICP-MS for simultaneous species interconversion correction and speciation analysis of Cr(III)/Cr(VI) in meat and dairy products

TALANTA

卷:222

Article

Saraiva, Marina^1,2  Chekri, Rachida¹  Leufroy, Axelle¹  Guerin, Thierry¹  Sloth, Jens J.²  Jitaru, Petru¹ 

[1] Univ Paris Est, ANSES, Lab Food Safety, F-94700 Maisons Alfort, France

[2] Tech Univ Denmark, Natl Food Inst, DK-2800 Lyngby, Denmark

关键词: Chromium speciation;    Species specific-isotope dilution;    HPLC-ICP-MS;    Foodstuffs;   

DOI  :  10.1016/j.talanta.2020.121538

来源: Elsevier

【 摘 要 】

This study presents the development, validation and application of a new analytical approach for the simulta-neous speciation analysis of Cr(III) and Cr(VI) in meat and dairy products by high-performance liquid chromatography (HPLC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) and double spike species specific-isotope dilution (SS-ID). The species extraction was achieved by sequential complexation of Cr(III) with ethylenediaminetetraacetic acid (EDTA) and of Cr(VI) with 1,5-diphenylcarbazide (DPC) in the same analytical run. The HPLC separation of complexed species was carried out using a short (5 cm) microbore anion-exchange HPLC column and a mobile phase consisting of 0.01 mol L-1 HNO3 + 2.5% (v/v) MeOH + 0.30 mol L-1 EDTA (pH = 2) in isocratic elution mode with excellent baseline separation achieved in less than 3 min. The method was validated by means of the accuracy profile approach by carrying out 6 measurement series in duplicate on (six) different days over a timespan of two months. The quantification limit was 0.013 mu g kg(-1) for Cr(III) and 0.049 mu g kg(-1) for Cr(VI), respectively. The measurement bias corresponding to the validity domain ranged from 0.01 to 0.11%, whereas the coefficient of variation in terms of repeatability (CVr) varied from 2.9 to 11.6% (depending on the analyte level) for Cr(III) and from 6.7 to 11.8% for Cr(VI). Similarly, the coefficient of variation in terms of intermediate reproducibility (CVR) ranged from 6.8 to 13% for Cr(III) and from 6.8 to 25.9% for Cr(VI), respectively. The method was successfully applied to the analysis of a selection of food samples such as baby and semi-skimmed milk and steak beef samples. Cr(VI) was not quantified in any of these samples while Cr(III) levels ranged between 2.7 and 4.7 mu g kg(-1), which were comparable with the levels of total chromium analysed in the same samples by ICP-MS (accredited method). The method presented here with combined use of species specific isotope dilution and sequential species complexation is a powerful analytical tool for accurate and precise quantification of Cr(III) and Cr(VI) at trace levels and allows for correction of any species inter conversion during sample preparation.

【 授权许可】

Free