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 Sep 11;14(9):631. doi: 10.3390/toxins14090631.
In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of deoxynivalenol, aflatoxin B, zearalenone, ochratoxin A, T-2 toxin and fumonisin B in feed and feedstuff was established. The sample was extracted with an acetonitrile-water mixture (60:40, /), purified by an immunoaffinity column, eluted with a methanol-acetic acid mixture (98:2, /), and reconstituted with a methanol-water mixture (50:50, /) after drying with nitrogen. Finally, the reconstituted solution was detected by LC-MS/MS and quantified by isotope internal standard method. The six mycotoxins had a good linear relationship in a certain concentration range, the correlation coefficients were all greater than 0.99, the limits of detection were between 0.075 and 1.5 µg·kg, and the limits of quantification were between 0.5 and 5 µg·kg. The average spike recoveries in the four feed matrices ranged from 84.2% to 117.1% with relative standard deviations less than 11.6%. Thirty-six actual feed samples were analyzed for mycotoxins, and at least one mycotoxin was detected in each sample. The proposed method is reliable and suitable for detecting common mycotoxins in feed samples.
本研究建立了一种同时测定饲料和饲料中脱氧雪腐镰刀菌烯醇、黄曲霉毒素 B、玉米赤霉烯酮、赭曲霉毒素 A、T-2 毒素和伏马菌素 B 的液相色谱-串联质谱（LC-MS/MS）方法。样品用乙腈-水混合物（60:40，/）提取，用免疫亲和柱净化，用甲醇-乙酸混合物（98:2，/）洗脱，氮气干燥后用甲醇-水混合物（50:50，/）重新溶解。最后，用 LC-MS/MS 检测重溶溶液，并采用同位素内标法定量。六种真菌毒素在一定浓度范围内具有良好的线性关系，相关系数均大于 0.99，检测限在 0.075 至 1.5 µg·kg 之间，定量限在 0.5 至 5 µg·kg 之间。四种饲料基质中六种真菌毒素的平均加标回收率在 84.2%至 117.1%之间，相对标准偏差均小于 11.6%。对 36 个实际饲料样品进行了真菌毒素分析，每个样品中至少检测到一种真菌毒素。该方法可靠，适用于检测饲料样品中的常见真菌毒素。
