Abstract

Rigorously standardized laboratory protocols are essential for meaningful comparison of data from multiple sites. Considering that interactions of minerals with organic matrices may vary depending on the material nature, there could be peculiar demands for each material with respect to digestion procedure. Acid digestion procedures were evaluated using different nitric to perchloric acid ratios and one- or two-step digestion to estimate the concentration of calcium, phosphorus, magnesium, and zinc in samples of carcass, bone, excreta, concentrate, forage, and feces. Six procedures were evaluated: ratio of nitric to perchloric acid at 2:1, 3:1, and 4:1 v/v in a one- or two-step digestion. There were no direct or interaction effects (p>0.01) of nitric to perchloric acid ratio or number of digestion steps on magnesium and zinc contents. Calcium and phosphorus contents presented a significant (p<0.01) interaction between sample type and nitric to perchloric acid ratio. Digestion solution of 2:1 v/v provided greater (p<0.01) recovery of calcium and phosphorus from bone samples than 3:1 and 4:1 v/v ratio. Different acid ratios did not affect (p>0.01) calcium or phosphorus contents in carcass, excreta, concentrate, forage, and feces. Number of digestion steps did not affect mineral content (p>0.01). Estimated concentration of calcium, phosphorus, magnesium, and zinc in carcass, excreta, concentrated, forage, and feces samples can be performed using digestion solution of nitric to perchloric acid 4:1 v/v in a one-step digestion. However, samples of bones demand a stronger digestion solution to analyze the mineral contents, which is represented by an increased proportion of perchloric acid, being recommended a digestion solution of nitric to perchloric acid 2:1 v/v in a one-step digestion.

Highlights

  • The ash content is a measure of the total amount of minerals present within a sample, whereas the mineral content is a measure of the amount of specific inorganic components, such as calcium (Ca), phosphorus (P), magnesium (Mg), and zinc (Zn), present within a sample

  • The objective of this study was to evaluate acid digestion procedures using different nitric to perchloric acid ratios and one- or two-step digestion to estimate the concentration of Ca, P, Mg, and Zn in samples of carcass, bone, excreta, concentrate, forages, and feces

  • When bone samples were evaluated, it was observed that the digestion solution of 2:1 v/v provided greater recovery of Ca and P than the 3:1 and 4:1 v/v ratio (p

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Summary

Introduction

The ash content is a measure of the total amount of minerals present within a sample, whereas the mineral content is a measure of the amount of specific inorganic components, such as calcium (Ca), phosphorus (P), magnesium (Mg), and zinc (Zn), present within a sample. Wet ashing is primarily used in the preparation of samples for subsequent analysis of specific minerals. It breaks down and removes the organic matrix surrounding the minerals through the use of both heat and acids, so that minerals are left in an aqueous solution. It has been demonstrated that analytical variability of a common diet among laboratories is large for Ca and Zn, representing twofold or more in the extremes, and considered intermediate for P (Cromwell et al, 2003). To minimize this possible bias, an accurate and standardized procedure should be used by different laboratories

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