Scientific Publications by FDA Staff

J AOAC Int 2017 Jul-Aug;100(4):1077-85

Multilaboratory validation of first action method 2016.04 for determination of four arsenic species in fruit juice by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry.

Kubachka K, Heitkemper DT, Conklin S

Before being designated AOAC First Action Official MethodSM 2016.04, the U.S. Food and Drug Administration’s method, EAM 4.10 High Performance Liquid Chromatography–Inductively Coupled Plasma–Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice, underwent both a single-laboratory validation and a multilaboratory validation (MLV) study. Three federal and five state regulatory laboratories participated in the MLV study, which is the primary focus of this manuscript. The method was validated for inorganic arsenic (iAs) measured as the sum of the two iAs species arsenite [As(III)] and arsenate [As(V)], dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) by analyses of 13 juice samples, including three apple juice, three apple juice concentrate, four grape juice, and three pear juice samples. In addition, two water Standard Reference Materials (SRMs) were analyzed. The method LODs and LOQs obtained among the eight laboratories were approximately 0.3 and 2 ng/g, respectively, for each of the analytes and were adequate for the intended purpose of the method. Each laboratory analyzed method blanks, fortified method blanks, reference materials, triplicate portions of each juice sample, and duplicate fortified juice samples (one for each matrix type) at three fortification levels. In general, repeatability and reproducibility of the method was ≤15% RSD for each species present at a concentration >LOQ. The average recovery of fortified analytes for all laboratories ranged from 98 to 104% iAs, DMA, and MMA for all four juice sample matrixes. The average iAs results for SRMs 1640a and 1643e agreed within the range of 96–98% of certified values for total arsenic.