SPIFAN Nutrients ERP Book_9-29-15

Fluor-02 SLV FOR ERP USE ONLY DO NOT DISTRIBUTE

Single Laboratory Validation for Fluoride Analysis in Infant Formula and Adult Nutritionals: AOAC SMPR 2014.016

Introduction

The purpose of this report is to document a single laboratory validation performed for the AOAC first action method for fluoride in infant formula and adult/ pediatric nutritional formula. The SPIFAN (stakeholder panel on infant formula and adult nutritionals) test material kit was used to determine that the method meets the standard method performance requirements (SMPRs) for linearity, limit of quantitation (LOQ), limit of detection (LOD), repeatability, and method accuracy.

Method:

Dionex ICS-5000 Reagent-Free HPIC System Dionex IonPac AS15, Analytical, 2 x 250 mm Dionex IonPac AG15, Guard, 2 x 50 mm

System

Columns

30˚C

Column Temperature

Dionex EGC 500 KOH cartridge with high pressure CR-ATC Gradient: 5 mM KOH (0-10 min), 5-35 mM KOH (10-12 min), 35 mM KOH (12-16 min), 60 mM KOH(16-30 min)

Eluent Source

Eluent condition

0.4 mL/min

Flow Rate

Injection Volume/Loop size 2.5 µL Inject Mode Push full Loop overfill factor 5

Suppressed conductivity with Dionex ERS 500 Electrolytically Regenerated Suppressor, recycle mode

Detection

60 mA

Suppresser Current System Backpressure

~2350 psi

~0.2 – 0.6 µS

Background Conductance

0.3 -0.8 nS/min peak-to-peak

Noise

30 min

Run Time

Samples

Determination of fluoride was conducted for the samples included in the SPIFAN test material kit. The matrixes are listed in Table 1.

Sample Preparation

1. Reconstituted powders

Step1: Place a 20 mL polypropylene bottle on the balance and tare it. Add 1.47 g of powder and record the weight.