Domijan Ana-Marija, Peraica Maja, Miletić-Medved Marica, Lucić Ana, Fuchs Radovan
Unit of Toxicology, Institute for Medical Research and Occupational Health, Ksaverska c. 2, 10000, Zagreb, Croatia.
J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Dec 25;798(2):317-21. doi: 10.1016/j.jchromb.2003.10.003.
This paper describes two different procedures for extraction of ochratoxin A (OTA) from urine samples: one using acidic chloroform-methanol mixture, followed by solid-phase extraction (SPE) clean-up and the other using commercial Chem Elut columns and a chloroform-formic acid mixture. The recovery of OTA using the procedure with silica gel columns was 82% with a R.S.D. < 8.4% and the detection and quantitation limits were 0.5 and 1.5 ng OTA/ml, respectively. The recovery of OTA in the second procedure with urine samples purified only on commercial Chem Elut columns was 95% with R.S.D. < 4.0%, and detection and quantitation limits 0.3 and 0.9 ng/ml, respectively. Both procedures of OTA extraction effectively eliminate interfering substances and give reliable and repeatable results. However, the procedure with Chem Elut columns gave higher recovery and lower detection and quantitation limits. It was successfully applied in determining OTA in human urine samples.
本文描述了从尿液样本中提取赭曲霉毒素A（OTA）的两种不同方法：一种是使用酸性氯仿 - 甲醇混合物，随后进行固相萃取（SPE）净化；另一种是使用商用Chem Elut柱和氯仿 - 甲酸混合物。使用硅胶柱的方法对OTA的回收率为82%，相对标准偏差（R.S.D.）< 8.4%，检测限和定量限分别为0.5和1.5 ng OTA/ml。在仅使用商用Chem Elut柱纯化尿液样本的第二种方法中，OTA的回收率为95%，R.S.D. < 4.0%，检测限和定量限分别为0.3和0.9 ng/ml。两种OTA提取方法均能有效消除干扰物质，并给出可靠且可重复的结果。然而，使用Chem Elut柱的方法具有更高的回收率以及更低的检测限和定量限。该方法已成功应用于测定人类尿液样本中的OTA。
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