采用免疫亲和柱净化和高效液相色谱法测定希腊产初榨橄榄油中的赭曲霉毒素A。

Determination of ochratoxin A in virgin olive oils of Greek origin by immunoaffinity column clean-up and high-performance liquid chromatography.

作者信息

Papachristou A, Markaki P

机构信息

Department of Food Chemistry, School of Chemistry, University of Athens, Greece.

出版信息

Food Addit Contam. 2004 Jan;21(1):85-92. doi: 10.1080/02652030310001632547.

DOI:10.1080/02652030310001632547

PMID:14744684

Abstract

An improved specific analytical method for ochratoxin A (OTA) determination in olive oil is described, using a methanolic-aqueous extraction, an immunoaffinity column clean up step and high-pressure liquid chromatography with fluorescence detection. The mean recovery was found at 108% (relative standard deviation, RSD = 4.7%) and the detection limit (DL) was estimated at 4.6 ng kg(-1). Along with OTA, aflatoxin B(1) (AFB(1)) was determined using the same extract. The recovery factor was 84.8% (RSD = 17.8%) and the DL was 56 ng kg(-1) olive oil. Both determinations were applied in 50 samples of olive oil originated from representative regions of Greece. Results revealed the presence of OTA in 88% of samples tested (n = 44, mean 267 ng kg(-1)). Among them, 10 were contaminated with more than 500 ng kg(-1) (median 568 ng kg(-1)), 10 with 200-500 ng kg(-1) (median 260 ng kg(-1)), 15 with 100-200 ng kg(-1) (median 140 ng kg(-1)), nine with DL-100 (median 60 ng kg(-1)) and in six samples, OTA was not detectable. Interestingly, most contaminated samples were from Southern Greece. Results of AFB(1) determination showed the presence of aflatoxin B(1) (60 ng kg(-1)) in only one olive oil sample also from Southern Greece. The levels of OTA found in Greek olive oil were relatively low as compared with other commodities such as cereals or wine reported in the literature.

摘要

本文描述了一种改进的用于测定橄榄油中赭曲霉毒素A（OTA）的特定分析方法，该方法采用甲醇 - 水萃取、免疫亲和柱净化步骤以及带荧光检测的高压液相色谱法。平均回收率为108%（相对标准偏差，RSD = 4.7%），检测限（DL）估计为4.6 ng kg⁻¹。除了OTA，还使用相同的提取物测定了黄曲霉毒素B₁（AFB₁）。回收率为84.8%（RSD = 17.8%），橄榄油中DL为56 ng kg⁻¹。这两种测定方法应用于来自希腊代表性地区的50个橄榄油样品。结果显示，在88%的测试样品（n = 44，平均267 ng kg⁻¹）中检测到OTA。其中，10个样品的OTA含量超过500 ng kg⁻¹（中位数为568 ng kg⁻¹），10个样品的含量在200 - 500 ng kg⁻¹之间（中位数为260 ng kg⁻¹），15个样品的含量在100 - 200 ng kg⁻¹之间（中位数为140 ng kg⁻¹），9个样品的含量在检测限 - 100 ng kg⁻¹之间（中位数为60 ng kg⁻¹），6个样品未检测到OTA。有趣的是，大多数受污染的样品来自希腊南部。AFB₁的测定结果显示，仅在一个同样来自希腊南部的橄榄油样品中检测到黄曲霉毒素B₁（60 ng kg⁻¹）。与文献报道的其他商品如谷物或葡萄酒相比，希腊橄榄油中发现的OTA水平相对较低。