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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