Multivariate Optimization of Conditions for Digestion of Wet Feeds for Dogs and Cats Using a Closed Digester Block and Multielement Determination by ICP-OES.

A full 24 factorial design was applied to find the best combination of diluted reagents (HNO3 and H2O2), time, and temperature for the digestion of samples of wet feed for dogs and cats using a closed digestion block. The residual carbon concentration (RCC) was used as the response in the factorial design. All variables and their interactions significantly influenced the digestion of the feed samples, as indicated by the RCC. The conditions established for the digestion of 0.05 g (dry mass) wet feed samples were the addition of 3.0 mol/L HNO3 and 5.0% m/m H2O2 in a final volume of 10 mL, followed by heating in a closed digestion block at a temperature of 170°C for 120 min. Analyses were performed by inductively coupled plasma (ICP) optical emission spectrometry (OES). LOQs ranged from 0.2 µg/g (Mg and Sr) to 51 µg/g (P). Accuracy of the analytical method was confirmed through the analysis of the Standard Reference Materials Tomato Leaves (NIST 1573), Apple Leaves (NIST 1515), and Peach Leaves (NIST 1547). The agreement values achieved ranged from 80.2 ± 0.3% for Ba to 113.8 ± 7.1% for Zn (n = 3). Addition and recovery tests were carried out by adding the analytes to a feed sample at two concentration levels, and the recoveries were between 84 ± 6 and 114 ± 10% for macroelements (Ca, K, Mg, and P; n = 3) and between 88 ± 3 and 113 ± 7% for microelements and trace elements (B, Cu, Fe, Sr, and Zn; n = 3). The precision values achieved for the different elements, expressed as RSDs, were better than 7.3% (Zn; n = 3) except for Cu determination, that was 14.6% (n=3). The optimized analytical method was applied to 10 commercial samples of wet feed for cats and dogs, with the concentrations of Al, B, Ba, Ca, Cu, Fe, K, Mg, Mn, P, Sr, and Zn determined by ICP-OES.

Multivariate optimization of an analytical method for the analysis of dog and cat foods by ICP OES.

Experimental design methodology was used to optimize an analytical method for determination of the mineral element composition (Al, Ca, Cd, Cr, Cu, Ba, Fe, K, Mg, Mn, P, S, Sr and Zn) of dog and cat foods. Two-level full factorial design was applied to define the optimal proportions of the reagents used for microwave-assisted sample digestion (2.0 mol L(-1) HNO3 and 6% m/v H2O2). A three-level factorial design for two variables was used to optimize the operational conditions of the inductively coupled plasma optical emission spectrometer, employed for analysis of the extracts. A radiofrequency power of 1.2 kW and a nebulizer argon flow of 1.0 L min(-1) were selected. The limits of quantification (LOQ) were between 0.03 µg g(-1) (Cr, 267.716 nm) and 87 µg g(-1) (Ca, 373.690 nm). The trueness of the optimized method was evaluated by analysis of five certified reference materials (CRMs): wheat flour (NIST 1567a), bovine liver (NIST 1577), peach leaves (NIST 1547), oyster tissue (NIST 1566b), and fish protein (DORM-3). The recovery values obtained for the CRMs were between 80 ± 4% (Cr) and 117 ± 5% (Cd), with relative standard deviations (RSDs) better than 5%, demonstrating that the proposed method offered good trueness and precision. Ten samples of pet food (five each of cat and dog food) were acquired at supermarkets in Aracaju city (Sergipe State, Brazil). Concentrations in the dog food ranged between 7.1 mg kg(-1) (Ba) and 2.7 g kg(-1) (Ca), while for cat food the values were between 3.7 mg kg(-1) (Ba) and 3.0 g kg(-1) (Ca). The concentrations of Ca, K, Mg, P, Cu, Fe, Mn, and Zn in the food were compared with the guidelines of the United States' Association of American Feed Control Officials (AAFCO) and the Brazilian Ministry of Agriculture, Livestock, and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento-MAPA).