A headspace solid-phase microextraction method of use in monitoring hexanal and pentane during storage: Application to liquid infant foods and powdered infant formulas

The determination of two secondary lipid oxidation compounds (hexanal and pentane) in liquid infant foods using a headspace solid-phase microextraction gas chromatographic (HS-SPME-GC) method has been developed and validated. The HS-SPME analytical conditions (fibre position, equilibration and sampling times) were selected. The analytical parameters of the method (linearity: hexanal from 2.48 to 84.78 ng/g, pentane from 6.21 to 79.55 ng/g; precision: hexanal 2.87%, pentane 2.343.46%; recovery: hexanal 106.60%, pentane 95.39%; detection limit: hexanal 3.63 ng and pentane 4.2 ng) demonstrate the usefulness of the method. Once optimized, the method was applied to liquid infant foods based on milk and cereals, and to powdered adapted and follow-up milk-based infant formulas (IF), stored for four and seven months. In all cases the hexanal content was higher in IF than in milk-cereal based infant foods. No pentane was found in IF

Limits of quantitation for laboratory assays

A common problem with laboratory assays is that a measurement of a substance in a test sample becomes relatively imprecise as the concentration decreases. A standard solution is to establish lower limits for reliable measurement. A quantitation limit is a level above which a measurement has sufficient precision to be reliably reported. The paper proposes a new approach to defining the limit of quantitation for the case where a linear calibration curve is used to estimate actual concentrations from measured values. The approach is based on the relative precision of the estimated concentration, using the delta method to approximate the precision. A graphical display is proposed for the assessment of estimated concentrations, as well as the overall reliability of the calibration curve. Our research is motivated by a clinical inhalation experiment. Comparisons are made between the approach proposed and two standard methods, using both real and simulated data. Copyright 2005 Royal Statistical Society.