Lima Liliane Spazzapam, Rossini Eduardo Luiz, Pezza Leonardo, Pezza Helena Redigolo
Instituto de Química, UNESP - São Paulo State University, R. Prof. Francisco Degni 55, P.O.Box 355, 14800-900 Araraquara, SP, Brazil.
Instituto de Química, UNESP - São Paulo State University, R. Prof. Francisco Degni 55, P.O.Box 355, 14800-900 Araraquara, SP, Brazil.
Spectrochim Acta A Mol Biomol Spectrosc. 2020 Feb 15;227:117774. doi: 10.1016/j.saa.2019.117774. Epub 2019 Nov 6.
This paper describes the development and application of a paper-based analytical device (μPAD) for the determination of hydrogen peroxide, an important adulterant in milk. The method employs the reaction between hydrogen peroxide and guaiacol, catalyzed by peroxidase, producing a red product, which is then quantified by digital imaging. Experimental design methodology was used to optimize the experimental conditions. The linear concentration range was from 12.5 × 10 to 150 × 10 mol L, resulting in the regression equation A = 0.02466 (±0.00192) + 17.053 (±0.750) C, with an excellent correlation coefficient (r = 0.986). The relative standard deviations obtained were 1.1 and 1.3% (intra-day), and 4.8 and 2.9% (inter-day), for 25.0 × 10 and 100 × 10 mol L of hydrogen peroxide, respectively. The limits of detection and quantification were 3.54 × 10 and 11.8 × 10 mol L, respectively, with standard deviation of the blank of 0.002012. The proposed method was successfully applied for the determination of peroxide in milk samples, with recoveries between 92.2 and 109%. The proposed device constitutes a valuable analytical tool for the identification of hydrogen peroxide adulteration and offers advantages including low cost, simplicity, portability, and no (or minimal) requirement for sample pretreatment.
本文描述了一种用于测定牛奶中重要掺假物过氧化氢的纸质分析装置(μPAD)的开发与应用。该方法利用过氧化氢与愈创木酚在过氧化物酶催化下的反应,生成红色产物,然后通过数字成像进行定量。采用实验设计方法优化实验条件。线性浓度范围为12.5×10至150×10 mol·L,得到回归方程A = 0.02466(±0.00192)+ 17.053(±0.750)C,相关系数极佳(r = 0.986)。对于25.0×10和100×10 mol·L的过氧化氢,日内相对标准偏差分别为1.1%和1.3%,日间相对标准偏差分别为4.8%和2.9%。检测限和定量限分别为3.54×10和11.8×10 mol·L,空白标准偏差为0.002012。该方法成功应用于牛奶样品中过氧化物的测定,回收率在92.2%至109%之间。所提出的装置是用于识别过氧化氢掺假的有价值分析工具,具有低成本、简单、便携以及对样品预处理要求低(或极少)等优点。