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Interlaboratory Validation of Modified Classical Qualitative Methods for Detection of Adulterants in Milk: Starch, Chloride, and Sucrose

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Abstract

Interlaboratory validation procedures were proposed and performed to confirm the effectiveness of modified classical qualitative methods for the detection of adulterants in milk, including starch, chloride, and sucrose, which were previously validated by a single laboratory approach. Raw milk samples that were adulterated with 150 g L−1 of water and 0.0, 0.3, 0.8, and 1.2 g L−1 of starch, 0, 1.5, 2.0, and 2.5 g L−1 of chlorides, and 0.0, 2.4, 3.0, and 3.6 g L−1 of sucrose were sent to 10 collaborators in Brazil that represent the government, food control, food industry, and university affiliations. Reliability rates of 93 to 100, 98 to 100, and 99 to 100 % were obtained for the starch, chlorides, and sucrose methods, respectively. The prediction intervals for the probability of detection proved the sensitivity and selectivity of the methods. Concordance values were greater than 0.85 to starch, 0.98 to chlorides, and 0.99 to sucrose, indicating precision and that the procedures were properly standardized between the collaborators. The estimated detection limits and unreliability regions confirmed the fitness of the modified methods for their respective purposes.

Interlaboratory validation of modified classical qualitative methods for detection of adulterants in milk

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Acknowledgments

The authors acknowledge the experimental farm of “Professor Hélio Barbosa” of the Veterinary School/Federal University of Minas Gerais State (EV/UFMG) for allowing the use of their facilities and animals during this project and for providing the raw cow milk samples. We acknowledge Pedro Paulo Borges Santos for his analytical assistance and the Brazilian agency “Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)” for financial support. The authors also express their appreciation to the collaborators for their participation in the study: GMO Centro de Pesquisas e Controle de Qualidade Ltda.; Hidrocepe Servicos de Qualidade Ltda. Epp; Ita Alimentos—Laticínios Ita Indústria e Comércio de Alimentos Ltda.; Itambé Alimentos S.A.; Laboratório de Análise Físico-Química em Alimentos do Laboratório de Química Agropecuária do Instituto Mineiro de Agropecuária (LAFQ/LQA/IMA); Laboratório de Química Bromatológica da Fundação Ezequiel Dias (FUNED); Laboratório Nacional Agropecuário de Minas Gerais do Ministério da Agricultura, Pecuária e Abastecimento (LANAGRO-MG/MAPA); Laboratório de Bromatologia—Unidade de Pesquisa Análise de Alimentos da Faculdade de Farmácia da Universidade Federal de Minas Gerais (BRO-UPAA/FAFAR/UFMG); NUGAP—Núcleo Global de Análise e Pesquisa Ltda.; and Trevo Alimentos—Nogueira e Rezende Indústria de Laticínio Ltda.

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Correspondence to Scheilla Vitorino Carvalho de Souza.

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Carina de Souza Gondim declares that she has no conflict of interest. Roberto Gonçalves Junqueira declares that he has no conflict of interest. Scheilla Vitorino Carvalho de Souza declares that she has no conflict of interest.

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de Souza Gondim, C., Gonçalves Junqueira, R. & Vitorino Carvalho de Souza, S. Interlaboratory Validation of Modified Classical Qualitative Methods for Detection of Adulterants in Milk: Starch, Chloride, and Sucrose. Food Anal. Methods 9, 2509–2520 (2016). https://doi.org/10.1007/s12161-016-0432-7

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