Rapid determination of sulfonamides in milk samples using fluorescence spectroscopy and class modeling with n-way partial least squares.
Rapid determination of sulfonamides in milk samples using fluorescence spectroscopy and class modeling with n-way partial least squares.
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DOI：
10.1016/j.aca.2006.12.038
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发表时间：
2007-03
影响因子：
6.2
通讯作者：
R. Diez;L. Sarabia;M. Ortiz
中科院分区：
文献类型：
--
作者：
R. Diez;L. Sarabia;M. Ortiz
本文提出了一种方法来评估的概率，假不遵守和假遵守的筛选方法，它给出了一阶或二阶多元信号。为了这项任务，120个样品的6种不同的牛奶已被测量的激发-发射荧光。样品中加入了不同量的三种磺胺类药物（磺胺嘧啶、磺胺甲基嘧啶和磺胺二甲嘧啶）。这些物质已被归类为指令96/23/EC附件I的B1组（兽药和污染物）。欧洲联盟（委员会条例EC编号281/96）已将肌肉、肝脏、肾脏和牛奶中总磺胺类药物的最大残留量（MRL）设定为100μ g/kg − 1。研究表明，激发-发射荧光光谱法结合偏最小二乘类模型（PLS-CM）方法是一种适用于牛奶中磺胺类药物总量检测的廉价方法。三个模型，PLS-CM，已建成，发射和激发光谱（一阶信号）和激发-发射矩阵（二阶信号）。在所有情况下，它都达到了第2002/657/EC号决定所要求的低于5%的错误遵守概率。在相同的荧光信号下，使用2-PLS、3-PLS和PARAFAC回归校正磺胺的总量。使用这种定量方法，对于5%的假不符合和假符合概率，MRL附近的检测能力CCβ估计为114.3 - 115.1μgkg− 1。
In this paper, a methodology to evaluate the probability of false non-compliance and false compliance for screening methods, which give first or second-order multivariate signals is proposed. For this task 120 samples of 6 different kinds of milk have been measured by excitation–emission fluorescence. The samples have been spiked with different amounts of three sulfonamides (sulfadiazine, sulfamerazine and sulfamethazine). These substances have been classified in group B1 (veterinary medicines and contaminants) of annex I of Directive 96/23/EC. The European Union (Commission Regulation EC no. 281/96) has set the maximum residue level (MRL) of total sulfonamides at 100μgkg−1in muscle, liver, kidney and milk. The work shows that excitation–emission fluorescence together with the partial least squares class modeling (PLS-CM) procedure may be a suitable and cheap screening method for the total amount of sulfonamides in milk. Three models, PLS-CM, have been built, for the emission and excitation spectra (first-order signals) and for the excitation–emission matrices (second-order signals). In all the cases it reaches probabilities of false compliance below 5% as required by Decision 2002/657/EC. With the same flourescence signals, the total quantity of sulfonamide was calibrated using 2-PLS, 3-PLS and PARAFAC regressions. Using this quantitative approach, the capability of detection, CCβ, around the MRL has been estimated between 114.3 and 115.1μgkg−1for a probability of false non-compliance and false compliance equal to 5%.