Plasencia J, Mirocha C J, Pawlosky R J, Smith J F
University of Minnesota, Department of Plant Pathology, St Paul 55108.
J Assoc Off Anal Chem. 1990 Nov-Dec;73(6):973-80.
The present paper describes a sensitive procedure for quantitative analysis of the Fusarium mycotoxins zearalenone and alpha-zearalenol in urine of ruminants. Extraction is done with an octadecyl (C18) column and cleanup with a silica column providing a preparation that is analyzed by gas chromatography-tandem mass spectrometry (GC-MS/MS). The trimethylsilyl ether derivatives of zearalenone and alpha-zearalenol yield molecular ions with m/z 462 and 536, respectively. These ions are selected in the first mass analyzer and then fragmented in a collision cell to give characteristic daughter ions (m/z 151, 333, 318, and 446). The method is known as multiple reaction monitoring (MRM). Elimination of chemical background noise by selecting proper fragment ions produces chromatograms in which identification and quantitation in a biological matrix is possible. The method was tested with sheep urine from an experimental feeding trial and was used to confirm natural mycotoxicosis of cows affected with zearalenone. Zearalenone (1 ppb) and alpha-zearalenol (14 ppb) were found in 2 different cow urine samples. The detection limit for both zearalenone and zearalenol is 1 ppb (1 ng/mL) in urine and is linear between 1 and 20 ppb for the former and 1 and 10 ppb for the latter.
本文描述了一种用于定量分析反刍动物尿液中镰刀菌霉菌毒素玉米赤霉烯酮和α-玉米赤霉醇的灵敏方法。用十八烷基（C18）柱进行萃取，并用硅胶柱进行净化，得到的提取物通过气相色谱-串联质谱（GC-MS/MS）进行分析。玉米赤霉烯酮和α-玉米赤霉醇的三甲基硅醚衍生物分别产生质荷比为462和536的分子离子。这些离子在第一个质量分析器中被选择，然后在碰撞池中裂解，产生特征性子离子（质荷比为151、333、318和446）。该方法称为多反应监测（MRM）。通过选择合适的碎片离子消除化学背景噪声，从而得到能够在生物基质中进行鉴定和定量的色谱图。该方法在一项实验性饲养试验的绵羊尿液中进行了测试，并用于确认受玉米赤霉烯酮影响的奶牛的天然霉菌毒素中毒情况。在两份不同的奶牛尿液样本中发现了玉米赤霉烯酮（1 ppb）和α-玉米赤霉醇（14 ppb）。玉米赤霉烯酮和玉米赤霉醇在尿液中的检测限均为1 ppb（1 ng/mL），前者在1至20 ppb之间呈线性，后者在1至10 ppb之间呈线性。
