State Key Laboratory of Animal Nutrition, College of Animal Science and Technology, China Agricultural University, Beijing 100193, China.
Clover Technology Group Inc., Beijing 100044, China.
Toxins (Basel). 2022 Nov 4;14(11):764. doi: 10.3390/toxins14110764.
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.
本研究建立了一种气相色谱-质谱联用(GC-MS)方法,用于检测饲料中的玉米赤霉烯酮及其五种衍生物,包括玉米赤霉烯酮、α-玉米赤霉烯醇、β-玉米赤霉烯醇、α-玉米赤霉烯醇和β-玉米赤霉烯醇。本方法采用免疫亲和柱对样品进行净化,然后对免疫亲和色谱分析后的洗脱液进行硅烷衍生化,最后用 GC-MS 进行分析。该方法通过玉米赤霉烯酮的同位素内标校正了基质效应。六种分析物在 2-500ng/mL 范围内具有良好的线性关系,相关系数均大于 0.99。检出限(LOD)和定量限(LOQ)均小于 1.5μg/kg 和 5.0μg/kg。六种饲料基质的平均加标回收率在 89.6%-112.3%之间,相对标准偏差(RSD)小于 12.6%。采用建立的方法对 20 个实际饲料样品进行了分析,至少检测到一个目标物。结果表明,所建立的 GC-MS 方法可靠,适用于饲料中玉米赤霉烯酮及其衍生物的测定。