Simões da Costa A M, Delgadillo I, Rudnitskaya A
CESAM and Chemistry Department, Aveiro University, Campus Universitario de Santiago, Aveiro 3810-193, Portugal.
QOPNA and Chemistry Department, Aveiro University, Campus Universitario de Santiago, Aveiro 3810-193, Portugal.
Talanta. 2014 Nov;129:63-71. doi: 10.1016/j.talanta.2014.04.030. Epub 2014 Apr 30.
An array of 10 potentiometric chemical sensors has been applied to the detection of total Fe, Cu, Pb and Cd content in digested wine. As digestion of organic matter of wine is necessary prior to the trace metal detection using potentiometric sensors, sample preparation procedures have been optimized. Different variants of wet and microwave digestion and dry ashing, 14 conditions in total, have been tested. Decomposition of organic matter was assessed using Fourier transform mid-infrared spectroscopy and total phenolic content. Dry ashing was found to be the most effective method of wine digestion. Measurements with sensors in individual solutions of Fe(III), Cu(II), Pb(II) and Cd(II) prepared on different backgrounds have shown that their detection limits were below typical concentration levels of these metals in wines and, in the case of Cu, Pb and Cd below maximum allowed concentrations. Detection of Fe in digested wine samples was possible using discrete iron-sensitive sensors with chalcogenide glass membranes with RMSEP of 0.05 mmol L(-1) in the concentration range from 0.0786 to 0.472 mmol L(-1). Low concentration levels of Cu, Pb and Cd in wine and cross-sensitivity of respective sensors resulted in the non-linearity of their responses, requiring back-propagation neural network for the calibration. Calibration models have been calculated using measurements in the model mixed solutions containing all three metals and a set of digested wine sample. RMSEP values for Cu, Pb and Cd were 3.9, 39 and 1.2 μmol L(-1) in model solutions and 2, 150 and 1 μmol L(-1) in digested wine samples.
采用一组10个电位型化学传感器检测消化葡萄酒中的总铁、铜、铅和镉含量。由于在使用电位型传感器检测痕量金属之前需要对葡萄酒中的有机物进行消化,因此对样品制备程序进行了优化。测试了湿法和微波消解以及干灰化的不同变体,总共14种条件。使用傅里叶变换中红外光谱和总酚含量评估有机物的分解情况。发现干灰化是葡萄酒消化最有效的方法。在不同背景下制备的铁(III)、铜(II)、铅(II)和镉(II)的单个溶液中使用传感器进行测量,结果表明它们的检测限低于葡萄酒中这些金属的典型浓度水平,对于铜、铅和镉,其检测限低于最大允许浓度。使用具有硫属化物玻璃膜的离散铁敏感传感器可以检测消化葡萄酒样品中的铁,在0.0786至0.472 mmol L(-1)的浓度范围内,RMSEP为0.05 mmol L(-1)。葡萄酒中铜、铅和镉的低浓度水平以及相应传感器的交叉敏感性导致其响应呈非线性,需要使用反向传播神经网络进行校准。使用包含所有三种金属的模型混合溶液和一组消化葡萄酒样品中的测量值计算校准模型。模型溶液中铜、铅和镉的RMSEP值分别为3.9、39和1.2 μmol L(-1),消化葡萄酒样品中分别为2、150和1 μmol L(-1)。