Simultaneous Determination of Arsenic, Cadmium, Mercury, and Lead in Raw Ingredients, Nutritional Products, and Infant Formula by Inductively Coupled Plasma Mass Spectrometry: Single-Laboratory Validation.

Abstract

A method was developed for the determination of As, Cd, Hg, and Pb in raw ingredients, nutritional products, and infant formula using inductively coupled plasma mass spectrometry (ICP-MS). Three raw ingredients (acid casein, maltodextrin, skim milk powder) and three standard reference materials [NIST 1548a (Typical Diet), NIST 1577c (Bovine Liver), NIST SRM 1568b (Rice Flour)] obtained from the National Institute of Standards and Technology were analyzed by two analysts using two ICP-MS instruments in different laboratories. NIST SRM 1568b was used as the control sample. All protocol validation parameters (intermediate precision, accuracy, linearity, quantitation limit, specificity, and robustness) were met. The overall precision (n = 8) for analyte concentrations (2.5-300 ng/g) ranged from 2 to 14% RSD. Spike recoveries ranged from 88 to109% for spike levels between 25 and 200%. The overall average concentration of As, Cd, Hg, and Pb measured in all three NIST SRMs were within the certified value ranges. Good linearity (correlation coefficient (r) = 0.9995 or better) was obtained for all analytes. Control chart results for 8 independent days showed that the method is robust (precision values of 10% and all points within ±3 σ were obtained). Excellent specificity was also demonstrated when the analytes were measured in the presence of high concentrations of the other concomitants.