title: Method validation for determination of arsenic, cadmium, chromium and lead in milk by means of dynamic reaction cell inductively coupled plasma mass spectrometry.
abstract: With Regulation No. 1881/2006 the European Union fixed a maximum level for lead in milk. Consequently, there is the need to determine very low concentration of elements that may be present in milk in trace and ultratrace levels. Quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS) combined with dynamic reaction cell (DRC) has been widely employed in order to reach very low concentration, requested for this product. Furthermore, the DRC technology can help in removing polyatomic and argon-based interferences. In the present study, a method for the determination of arsenic, cadmium, chromium and lead in bovine milk was validated according to the EU common standards by means of DRC-ICP-MS. The main parameters evaluated in the validation were: recovery, repeatability and within-laboratory reproducibility, detection and quantification limits, linearity range and measurement uncertainty. Additionally, stability studies of the analyte in solution and ruggedness studies were carried out. The results obtained for limit of detection (LoD) and limit of quantification (LoQ) in microg kg(-1) were respectively: As, 3.1 and 9.5; Cd, 0.08 and 0.24; Cr, 0.229 and 0.693; Pb, 0.5 and 1.5. While for the recovery: As, 91%; Cd 96%; Cr 99%; Pb, 95%. As for the repeatability: As, 7%; Cd, 3%; Cr, 6%; Pb, 4%.
authors.affiliation: Department of Environment and Primary Prevention, Istituto Superiore di Sanità, Viale Regina Elena 299, Rome, Italy. sonia.dilio@iss.it
authors.forename: S
authors.initials: S
authors.lastname: D'Ilio
authors.forename: F
authors.initials: F
authors.lastname: Petrucci
authors.forename: M
authors.initials: M
authors.lastname: D'Amato
authors.forename: M
authors.initials: M
authors.lastname: Di Gregorio
authors.forename: O
authors.initials: O
authors.lastname: Senofonte
authors.forename: N
authors.initials: N
authors.lastname: Violante
mesh_terms: D000818:Animals; D001151:Arsenic / Q000032:analysis*; D002104:Cadmium / Q000032:analysis*; D002138:Calibration; D002857:Chromium / Q000032:analysis*; D005062:European Union; D005506:Food Contamination / Q000032:analysis*; D006801:Humans; D041943:Infant Formula / Q000737:chemistry; D007854:Lead / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods; D008892:Milk / Q000737:chemistry*; D008895:Milk, Human / Q000737:chemistry; D015203:Reproducibility of Results
chemical_list: D002104:Cadmium; D002857:Chromium; D007854:Lead; D001151:Arsenic