Abstract
A method was developed to determine 27 elements (aluminum, arsenic, boron, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, mercury, molybdenum, nickel, phosphorus, potassium, selenium, sodium, sulfur, vanadium, zinc, antimony, uranium, beryllium, thallium, and thorium) in animal feeds and pet foods using closed vessel microwave digestion and inductively coupled plasma-massspectrometry. These elements can adversely affect animal health when amounts become excessive or deficient in food. For potentially toxic elements, the target LOQ was determined to be 1/10 the lowest maximum tolerable level (MTL) for the most sensitive animal species. For nutritionally essential elements,the target LOQ was determined to be 1/10 the concentration that would be considered deficient in feed if that level is lower than 1/10 the lowest MTL. The targeted high end of the quantitation range wasselected as twice the highest MTL. A single-laboratory validation (SLV) was performed to determine theaccuracy and precision of the method, and the resultswere evaluated with respect to predetermined performance characteristics. The test materials used in the SLV included two National Institute of Standardsand Technology certified reference materials, two Association of American Feed Control Officials (AAFCO) check samples, and one in-house previously analyzed feed sample. The concentrations of each elementdetermined were the result of spiked analyte,incurred analyte, or a combination of spiked and incurredanalyte. All samples were analyzed seven times on different days at 2 × LOQ and at the midrangeconcentration. For most data, the results of the SLV met or exceeded the criteria for accuracy and repeatability. For accuracy, K at the midrange level had a mean recovery of 95%, which is just below the low preferred accuracy threshold of 97%. For repeatability, all the 2 × LOQ CVr values were below the preferred values. Be, Cr, Ni, Na,Mn, and S all had midrange CVr values exceeding the preferred values. Be had the highest midrange CVr value of 9.93. Eight AAFCO check samples were also analyzed to determine the method’s accuracy and repeatability for elements at the manufacturer’s claimed levels. For accuracy, all results had z-scores <1.5. For repeatability, three CVr values from two AAFCO check samples were greater than the preferred limits.
Trace Metal Content and Availability of Essential Metals in Agricultural Soils of Alicante (Spain)