Abstract：
In this study, a gas chromatography-mass spectrometry (GC-MS) method was established for the determination of zearalenone and its five derivatives in feed, including zearalanone, α-zearalanol, β-zearalanol, α-zearalenol, and β-zearalenol. An effective immunoaffinity column was prepared for sample purification, which was followed by the silane derivatization of the eluate after an immunoaffinity chromatography analysis for target compounds by GC-MS. Matrix effects were corrected by an isotope internal standard of zearalenone in this method. The six analytes had a good linear relationship in the range of 2-500 ng/mL, and the correlation coefficients were all greater than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) were less than 1.5 μg/kg and 5.0 μg/kg, respectively. The average spike recoveries for the six feed matrices ranged from 89.6% to 112.3% with relative standard deviations (RSDs) less than 12.6%. Twenty actual feed samples were analyzed using the established method, and at least one target was detected. The established GC-MS method was proven to be reliable and suitable for the determination of zearalenone and its derivatives in feed.
摘要：
在这项研究中,建立了饲料中玉米赤霉烯酮及其5种衍生物的气相色谱-质谱(GC-MS)测定方法,包括玉米赤霉酮,α-玉米赤霉烷醇,β-玉米赤霉烷醇，α-玉米赤霉烯醇，和β-玉米赤霉烯醇。制备了有效的免疫亲和柱用于样品纯化，在通过GC-MS对目标化合物进行免疫亲和层析分析后，对洗脱液进行硅烷衍生化。在此方法中，通过玉米赤霉烯酮的同位素内标校正了基体效应。6种分析物在2-500ng/mL范围内具有良好的线性关系,相关系数均大于0.99。检测限(LODs)和定量限(LOQs)分别小于1.5μg/kg和5.0μg/kg,分别。六个饲料基质的平均加标回收率为89.6％至112.3％，相对标准偏差（RSD）小于12.6％。使用建立的方法对20个实际饲料样品进行了分析，并且至少检测到一个目标。所建立的气相色谱-质谱联用方法可靠,适用于饲料中玉米赤霉烯酮及其衍生物的测定。
