Determination of total fat in milk- and soy-based infant formula powder by supercritical fluid extraction - PVM 2:2002

Abstract

Commercially available simple benchtop systems using CO2 supercritical fluid extraction (SFE) eliminate expensive organic solvent disposal problems and offer potential to meet a demand for rapid, accurate high-volume gravimetric determinations of total fat content of infant formula powders. A Data Quality Objectives (DQOs) approach was used to evaluate the performance characteristics of instrumental SFE extraction for determination of total gravimetric fat in infant formula. The established DQOs included the following: Accuracy.-Correct values were obtained for a suitable reference material, SRM 1846 Infant Formula [National Institute of Standards and Technology (NIST), Gaithersburg, MD]. Ruggedness.-Variables were defined as (1) extraction time (35 min optimum); (2) ratio of sample size to diatomaceous earth support material (1 g sample/2 g support); (3) ratio of distilled water to alcohol (50% isopropanol optimum for both milk- and soy-based infant formula samples); (4) extraction flow rate was 3-3.5 mL/min optimum. Precision.-Relative standard deviations of multiple determinations fell within the Horwitz limits of acceptability of ≤2.8 % at the level of analyte determined (0.34-2.5% obtained). Scope of applicability.-Includes milk- and soy-based infant formula powders. Research data were obtained by use of a commercially available fat analyzer. Samples of the SRM, 2 commercial milk-based and 3 commercial soy-based infant formula products were distributed to 2 additional collaborating laboratories. Very good agreement was obtained among the submitting and collaborating laboratories for these samples. The use of clearly defined DQOs to establish method performance characteristics, along with the commercially available reference material, provided the mechanism for verification and validation of analytical methodology.