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免疫亲和柱净化-同位素稀释气相色谱-质谱法测定饲料中玉米赤霉烯酮及其衍生物

Determination of Zearalenone and Its Derivatives in Feed by Gas Chromatography-Mass Spectrometry with Immunoaffinity Column Cleanup and Isotope Dilution.

机构信息

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.

出版信息

Toxins (Basel). 2022 Nov 4;14(11):764. doi: 10.3390/toxins14110764.

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

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。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/440e/9697342/d0f5e5f28ac8/toxins-14-00764-g001.jpg

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