Tabata Setsuko, Iida Kenji, Kimura Keisuke, Iwasaki Yumiko, Nakazato Mitsuo, Kamata Kunihiro, Hirokado Masako
Tokyo Metropolitan Institute of Public Health, Tokyo, Japan.
Shokuhin Eiseigaku Zasshi. 2008 Apr;49(2):100-5. doi: 10.3358/shokueishi.49.100.
Methods using high-performance liquid chromatography with fluorescence detection (HPLC-FL) and using liquid chromatography with tandem mass spectrometry (LC/MS/MS) were developed for simultaneous determination of ochratoxin A (OTA), ochratoxin B (OTB) and citrinin (CIT) in cereal, fruit, and coffee products. The samples were extracted with ethyl acetate under an acidic condition, and then cleaned up with liquid-liquid separation. The test solutions were analyzed by reverse-phase HPLC-FL and LC/MS/MS. Mass spectral acquisition was performed in positive ion mode by applying multiple reaction monitoring. The performances of both detectors were almost equivalent. The recoveries of OTA and OTB were 87-111%, and that of CIT were 70-88%. The limits of quantification (S/N> or =10) of OTA, OTB and CIT was 0.1 mug/kg or less. These methods were considered to be useful for the determination of the three mycotoxins at low levels (0.1 microg/kg).
建立了采用高效液相色谱-荧光检测法(HPLC-FL)和液相色谱-串联质谱法(LC/MS/MS)同时测定谷物、水果和咖啡产品中赭曲霉毒素A(OTA)、赭曲霉毒素B(OTB)和桔霉素(CIT)的方法。样品在酸性条件下用乙酸乙酯萃取,然后通过液-液分离进行净化。测试溶液采用反相HPLC-FL和LC/MS/MS进行分析。通过多反应监测在正离子模式下进行质谱采集。两种检测器的性能几乎相当。OTA和OTB的回收率为87%-111%,CIT的回收率为70%-88%。OTA、OTB和CIT的定量限(S/N≥10)为0.1μg/kg或更低。这些方法被认为对于低水平(0.1μg/kg)的三种霉菌毒素的测定是有用的。