Ishii Rie, Takahashi Kunihiko, Matsumoto Ryuji
Saitama Prefectural Institute of Public Health, Sakura-ku, Saitama, Japan.
Shokuhin Eiseigaku Zasshi. 2011;52(1):34-9. doi: 10.3358/shokueishi.52.34.
A simple method using high-performance liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was investigated for the detection of the antiprotozoal drug imidocarb in 10 livestock and seafood products. Liquid chromatographic separation employed a TSK VMpak-25 column with ammonium acetate-acetonitrile as a mobile phase. Mass spectral acquisition was performed in the ESI positive-ion mode. Imidocarb was extracted from all samples using liquid extraction with acetonitrile under basic conditions. For samples other than honey, fat-soluble impurities were removed by acetonitrile-hexane partitioning. The salting-out technique was used for extraction from honey in order to improve the separation of the organic solvent and water added to the honey sample. The limit of quantitation was 0.005 µg/g (expressed as concentration in samples). The recoveries from all samples were 76-109%, and the repeatability and reproducibility were also satisfactory.
研究了一种使用高效液相色谱-串联质谱联用（LC-MS/MS）的简单方法，用于检测10种畜禽和海产品中的抗原虫药物咪唑苯脲。液相色谱分离采用TSK VMpak-25柱，以醋酸铵-乙腈为流动相。质谱采集在电喷雾电离正离子模式下进行。在碱性条件下，使用乙腈液液萃取从所有样品中提取咪唑苯脲。对于蜂蜜以外的样品，通过乙腈-己烷分配去除脂溶性杂质。采用盐析技术从蜂蜜中提取，以改善添加到蜂蜜样品中的有机溶剂和水的分离。定量限为0.005 µg/g（以样品中的浓度表示）。所有样品的回收率为76%-109%，重复性和再现性也令人满意。
