固相萃取柱净化-超高效液相色谱-串联质谱法快速测定液态乳中14 种真菌毒素

建立使用固相萃取柱净化液态乳中14 种真菌毒素（黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B1、伏马毒素B2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸）多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取，固相萃取柱Oasis PRiME HLB净化后，以0.1%甲酸溶液与乙腈为流动相，经ACQUITY UPLC HSS T3色谱柱（2.1?mm×100?mm，1.8?μm）分离，梯度洗脱，采用电喷雾-正离子多反应监测模式，外标法定量。结果表明：14?种真菌毒素的定量限（RSN≥10）为0.5～5?μg/kg，高、中、低3?个添加水平时，平均回收率为67.7%～112.7%，相对标准偏差为0.43%～7.28%。该方法的检测速度快，净化效果较好，基质干扰较少，灵敏度高，结果准确、可靠，可用于液态乳中真菌毒素的检测分析。

Determination of 14 Mycotoxins in Liquid Milk by Solid-Phase Extraction Coupled with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

A rapid method was established for detecting 14 mycotoxins (aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, aflatoxin M1, ochratoxin A, citrinin, T-2 toxin, sterigmatocystin, fumonisin B1, fumonisin B2, zearalenone, deoxynivalenol, and penicillic acid) in liquid milk by solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were defatted and extracted with 0.1% formic acid acetonitrile and the extract was cleaned up with Oasis PRiME HLB solid-phase extraction column. The analytes were separated on HSS T3 column (2.1 mm × 100 mm, 1.8 μm) with a mobile phase composed of 0.1% formic acid and acetonitrile using gradient elution. Detection was carried out by tandem mass spectrometry using positive ionization in the multiple-reaction monitoring (MRM) mode. An external standard method was applied for quantification. Results showed that the limits of quantitation (LOQs) of 14 mycotoxins in matrices were between 0.5 and 5 μg/kg. Average recoveries at 3 different spiked levels were 67.7%–112.7% with relative standard deviation (RSD) of 0.43%–7.28%. With the advantages of rapidity, high purification efficiency, low matrix interference and accurate and reliable results, the method is useful for the analysis of mycotoxins in liquid milk.