Accurate Determination of Lead in Different Dairy Products by Graphite Furnace Atomic Absorption Spectrometry

Milk is one of the basic food groups in the human diet, both in its original form and as various dairy products. The Chinese contaminated baby formula scandal in 2008 has increased public awareness of contamination possibilities, and has lead to tighter supervision of dairy products as China is faced with demands – both from home and abroad – to improve its food safety record. It is well-known that lead (Pb) is toxic and causes damage to the nervous system; it has a particularly detrimental effect on young children1 and it has become a cause of major concern since the 1970s. As per World Health Organization (WHO) standards, the permissible limit of lead in drinking water is 10 μg/kg (parts per billion, ppb). Following an in-depth review of the toxicological literature, the Chinese guideline for maximum levels of lead content is set at 20 μg/kg (ppb wet weight) in infant formula (use of milk as a raw material measured by fluid milk diluted from powder, referring to the product ready-to-use) and at 50 μg/kg (ppb) in fresh milk, respectively.2

Lead analysis has traditionally been one of the major applications of graphite furnace atomic absorption spectrometry (GFAAS) worldwide. Currently, the Chinese regulatory framework approved standard methods for lead analysis has set GFAAS as the technique for the compulsory arbitration in food testing.3 In order to ensure protection of consumers, analysis should be sensitive, efficient, and cost-effective so that more effective monitoring can be accomplished. Because GFAAS is a mature technique, it is well-understood and routinely used by technicians and suitable for this determination. Sample preparation is an important part of an analysis and yet can be time consuming.

Generally, milk is an emulsion or colloid of butterfat globules within a water-based fluid. The exact components of raw milk vary by different animal species, but it contains significant amounts of lactose, fat, protein and minerals as well as vitamins. Due to the relative interference resulting from such a complex matrix, complete decomposition of milk samples prior to instrumental measurement by microwave or heating block acid digestion is generally recommended. This approach, however, is more time-consuming and poses a more rigorous requirement on quality assurance than simple dilution when concentrations of lead are to be determined at μg/kg level in the final solution which is extremely sensitive to reagent blank contribution and environmental contamination.

To overcome these issues, this work describes a simple and direct dilution method for sample preparation, followed by automated analysis using GFAAS. This method minimizes sample preparation, and also reduces potential contamination while still maintaining the speed of analysis.

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