Department of Pharmacology, Faculty of Veterinary Medicine, Kasetsart University, Bangkok 10900, Thailand.
Oil Crops Research Institute of the Chinese Academy of Agricultural Sciences, Wuhan 430062, China.
Toxins (Basel). 2020 Apr 13;12(4):253. doi: 10.3390/toxins12040253.
A reliable, sensitive and accurate multiple mycotoxin method was developed for the simultaneous determination of 17 mycotoxins in swine, poultry and dairy feeds using stable isotope dilution (C-ISTD) and (ultra)-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A simple QuEChERS-based method (quick, easy, cheap, effective, rugged and safe) was developed consisting of soaking with a solution of 1% formic acid followed by extraction with acetonitrile, clean-up with C18 sorbent and finally adding C-ISTD before the UHPLC-MS/MS analysis. The chromatographic condition was optimized for separation and detection of the 17 mycotoxins using gradient elution. The method's performance complied with the SANTE/11813/2017 standard and had mean recovery accuracies in the range 70%-120% and precision testing of % relative standard deviation (RSD) £ 20%. The limit of detection and limit of quantification values ranged from 0.25 to 40.0 ng/g and 0.5 to 100.0 ng/g, respectively. Finally, the method was applied to analyze feed samples, with the results showing that fumonisins, zearalenone, aflatoxin B1 and deoxynivalenol were the most prevalent mycotoxins contaminating the feed samples.
建立了一种可靠、灵敏、准确的多真菌毒素分析方法，采用同位素稀释（C-ISTD）和（超）高效液相色谱-串联质谱（HPLC-MS/MS），可同时测定猪、禽和奶牛饲料中的 17 种真菌毒素。本研究建立了一种简单的基于 QuEChERS 的方法（快速、简单、廉价、有效、耐用和安全），包括用 1%甲酸溶液浸泡，然后用乙腈提取，用 C18 吸附剂净化，最后在 UHPLC-MS/MS 分析前加入 C-ISTD。采用梯度洗脱优化了 17 种真菌毒素的色谱分离和检测条件。该方法的性能符合 SANTE/11813/2017 标准，平均回收率在 70%-120%范围内，相对标准偏差（RSD）%精度测试£20%。检测限和定量限范围分别为 0.25-40.0ng/g 和 0.5-100.0ng/g。最后，该方法应用于饲料样品分析，结果表明，伏马菌素、玉米赤霉烯酮、黄曲霉毒素 B1 和脱氧雪腐镰刀菌烯醇是污染饲料样品的最常见真菌毒素。
