National Institute of Health Sciences, 1-18-1 Kamiyoga, Setagaya-ku, Tokyo 158-8501, Japan.
Rapid Commun Mass Spectrom. 2010 Aug 30;24(16):2445-52. doi: 10.1002/rcm.4663.
A method for the simultaneous quantitative determination of deoxynivalenol (DON), T-2 toxin (T-2), HT-2 toxin (HT-2) and zearalenone (ZEN) in wheat and biscuit by liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) coupled with immunoaffinity extraction is described. A clean-up was carried out using a DZT MS-PREP immunoaffinity column (IAC), and the effect of the sample dilution rate and sample loading was investigated. Furthermore, the effects of ion suppression of a multifunctional column (MFC) and the IAC in the clean-up were compared. The results with the DZT MS-PREP IAC showed that it is possible to make the sample dilution rate low, and indicated a higher solvent-tolerance than usual with an IAC. Sample loading was optimized at 0.25 g. Ion suppression was lowered by purification of the toxins using the DZT MS-PREP IAC. Recoveries of each mycotoxin from wheat and biscuit samples spiked at two levels ranged from 78 to 109%. The limits of detection in wheat and biscuit was in the range of 0.03-0.33 ng x g(-1). From these studies, it is suggested that use of an IAC is effective in the clean-up of each mycotoxin, and, when combined with LC/ESI-MS/MS, it is good for the determination of mycotoxins in foodstuffs due to its rapidity and high sensitivity.
本文描述了一种采用液相色谱/电喷雾串联质谱（LC/ESI-MS/MS）联用免疫亲和萃取技术同时定量检测小麦和饼干中脱氧雪腐镰刀菌烯醇（DON）、T-2 毒素（T-2）、HT-2 毒素（HT-2）和玉米赤霉烯酮（ZEN）的方法。采用 DZT MS-PREP 免疫亲和柱（IAC）进行净化，并考察了样品稀释率和上样量的影响。此外，还比较了多功能柱（MFC）和 IAC 对离子抑制的影响。结果表明，DZT MS-PREP IAC 可使样品稀释率降低，且对 IAC 具有较高的溶剂耐受性。优化的上样量为 0.25 g。采用 DZT MS-PREP IAC 对毒素进行净化，可降低离子抑制。从小麦和饼干加标样品中各真菌毒素的回收率为 78%109%。在小麦和饼干中的检测限为 0.030.33ng·g-1。研究表明，IAC 对各真菌毒素的净化效果良好，与 LC/ESI-MS/MS 联用，由于其快速、高灵敏度，适用于食品中真菌毒素的检测。
