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Single Laboratory Validation for Fluoride and Chloride 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 and chloride 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:

System

Dionex ICS-5000 Reagent-Free HPIC System

Columns

Dionex IonPac AS15, Analytical, 2 x 250 mm

Dionex IonPac AG15, Guard, 2 x 50 mm

Column Temperature

30˚C

Eluent Source

Dionex EGC 500 KOH cartridge with high pressure CR-ATC

Eluent condition

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)

Flow Rate

0.4 mL/min

Injection Volume/Loop size

2.5 μL

Inject Mode

Push full

Loop overfill factor

5

Detection

Suppressed conductivity with Dionex ERS 500 Electrolytically

Regenerated Suppressor, recycle mode

Suppresser Current

60 mA

System Backpressure

~2350 psi

Background Conductance

~0.2

0.6 μS

Noise

0.3 -0.8 nS/min peak-to-peak

Run Time

30 min

Samples

Determination of fluoride and chloride 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 2.50 g of

powder and record the weight.

Fluor-02/Chlor-03 (February 2016)

FOR ERP USE ONLY

DO NOT DISTRIBUTE