Vatinno Rosa, Aresta Antonella, Zambonin Carlo G, Palmisano Francesco
Dipartimento di Chimica, Università degli Studi di Bari, Via E. Orabona, 4, I-70126 Bari, Italy.
J Chromatogr A. 2008 Apr 11;1187(1-2):145-50. doi: 10.1016/j.chroma.2008.02.020. Epub 2008 Feb 12.
A new method for the determination of Ochratoxin A (OTA) in green coffee beans by solid-phase microextraction (SPME) coupled to liquid chromatography with fluorescence detection (LC-FD) is described for the first time. Coffee samples were extracted by a 5% NaHCO(3) solution, followed by a clean-up step of the extract by chloroform partition. The aqueous extract was then acidified and finally subjected to SPME-LC-FD analysis. The investigated linear range in coffee was 2-32 ng/g. Within-day RSD% in coffee spiked at 2 and 32 ng/g levels were 3.3 and 2.7, respectively, whereas the between-days RSD% were 4.1 and 3.8, respectively. The limits of detection (LOD) and quantitation (LOQ), calculated at a signal-to-noise ratio of 3 and 10 (noise calculated peak to peak on a blank chromatogram at the OTA retention time), were 0.3 and 2 ng/g, respectively.
首次描述了一种通过固相微萃取（SPME）结合液相色谱荧光检测（LC-FD）测定生咖啡豆中赭曲霉毒素A（OTA）的新方法。咖啡样品用5%的NaHCO₃溶液萃取，然后通过氯仿分配对萃取物进行净化步骤。接着将水相萃取物酸化，最后进行SPME-LC-FD分析。在咖啡中研究的线性范围为2 - 32 ng/g。在添加水平为2和32 ng/g的咖啡中，日内相对标准偏差（RSD%）分别为3.3和2.7，而日间RSD%分别为4.1和3.8。在OTA保留时间处，以空白色谱图上峰峰噪声比为3和10计算的检测限（LOD）和定量限（LOQ）分别为0.3和2 ng/g。
