Validation of two analytical methods for the determination of ochratoxin A by reversed-phased high-performance liquid chromatography coupled to fluorescence detection in musts and sweet wines from Andalusia
Validation of two analytical methods for the determination of ochratoxin A by reversed-phased high-performance liquid chromatography coupled to fluorescence detection in musts and sweet wines from Andalusia
复制标题
DOI：
10.1016/j.aca.2006.02.002
复制
发表时间：
2006-04-27
影响因子：
6.2
通讯作者：
Barroso, CG
中科院分区：
文献类型：
--
作者：
Hernández, MJ;García-Moreno, MV;Barroso, CG
一些西班牙甜酒是用葡萄干制成的，葡萄干是采摘后直接暴露在阳光下干燥的葡萄。这种干燥过程可以促进赭曲霉毒素A(OTA)的形成。Ota是一种由几种真菌形成的真菌毒素。它与人类的肾病有关，在人类身上可能有很长的半衰期。本研究的目的是建立和应用两种分析方法，分别用于分析葡萄汁(在葡萄干过程中)和甜酒中OTA。两种分析方法均采用反相高效液相色谱与荧光检测相结合的方法。在GRPE MASH中，该方法包括将样品直接注入到高效液相-毛细管气相色谱系统中，而不需要任何事先的清理程序。甜酒样品的复杂性要求在C18柱上进行固相萃取(SPE)净化，使OTA能够从基质中分离出来。对所用方法进行了统计验证。验证还包括用标准获得的曲线斜率与通过增加标准获得的回归曲线的比较。对标准添加进行了两种不同的研究。其中一种方法在没有样品制备的情况下得到了验证，并应用于必须样品的测定。另一种方法用固相萃取进行验证，并应用于甜酒样品的分析。回收率始终在89.69%以上。方法检出限(S/N=3)和定量限(S/N=10)分别为0.22和0.77亩/升(-1)。总体而言，获得的分析数据在p，g L(-1)以下的浓度水平上提供了良好的结果。(C)2006爱思唯尔B.V.保留所有权利。
Some Spanish sweet wines are made from raisins, grapes dried by direct exposure to the sun after picking. This drying process can encourage ochratoxin A (OTA) formation. OTA is a mycotoxin formed by several fungi. It has been linked to nephropathy in humans, and may have a long half-life in humans. The aim of this study is to develop and to apply two procedures for the analysis of OTA in grape musts (during the raisining process) and sweet wines, respectively. Reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to fluorescence detection (FLD) was employed in both analytical methods. In grape must, the method involves the direct injection of the sample in a HPLC-FLD system without any kind of prior clean-up procedure. The complexity of the sweet wine samples requires a solid-phase extraction (SPE) clean-up on a C18 column which enables the OTA to be isolated from the matrix. The methods used were statistically validated. The validation also included the comparison of the slopes of the curve obtained with standards and the regression curves obtained by the addition of a standard. Two different studies of standard additions were conducted. One method was validated without sample preparation and it was applied to must samples. The other method was validated with SPE extraction and it was applied to sweet wine samples. Recovery was always better than 89.69%. The limit of detection (S/N=3) and limit of quantification (S/N= 10) were established at 0.22 and 0.77 mu gl(-1), respectively. In general, the analytical data obtained provided good results at the sub-p,g l(-1) concentration level. (c) 2006 Elsevier B.V. All rights reserved.