Monaci L, Palmisano F, Matrella R, Tantillo G
Dipartimento di Chimica, Università di Bari, Via Orabona 4, 70126 Bari, Italy.
J Chromatogr A. 2005 Oct 7;1090(1-2):184-7. doi: 10.1016/j.chroma.2005.07.020.
A fast high-performance liquid chromatography method has been devised for the determination of ochratoxin A (OTA) in Italian salami in the low part-per-trillion (pg/g) level. The samples were extracted with ethyl acetate and purified by immunoaffinity column (IAC). The IAC eluate could be directly injected or previously concentrated 10-fold. Recovery at 0.5 and 1 ng/g was 77 +/- 4%. The between-day coefficient of variation measured over 5 days on samples spiked at 1 ng/g was 8%. The developed method required a relatively small volume of non-halogenated organic solvent and the whole procedure was simpler and faster compared to other existing procedures. The limit of detection was 0.06 ng/g that could be even lowered using a preconcentration step. A total of 30 salami samples were analysed using this procedure; the most contaminated sample was found to have OTA concentration at 0.4 ng/g level.
已设计出一种快速高效液相色谱法，用于测定意大利萨拉米香肠中低至万亿分之一（皮克/克）水平的赭曲霉毒素A（OTA）。样品用乙酸乙酯萃取，并用免疫亲和柱（IAC）纯化。IAC洗脱液可直接进样或预先浓缩10倍。0.5和1纳克/克水平的回收率为77±4%。在5天内对加标量为1纳克/克的样品进行的日间变异系数为8%。所开发的方法所需的非卤代有机溶剂体积相对较小，与其他现有方法相比，整个过程更简单、更快。检测限为0.06纳克/克，使用预浓缩步骤甚至可以降低。使用该方法共分析了30个萨拉米香肠样品；发现污染最严重的样品中OTA浓度为0.4纳克/克水平。
