Simultaneous determination of multi-mycotoxins in palm kernel cake (PKC) using liquid chromatography-tandem mass spectrometry (LC-MS/MS)
Simultaneous determination of multi-mycotoxins in palm kernel cake (PKC) using liquid chromatography-tandem mass spectrometry (LC-MS/MS)
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DOI：
10.1080/19440049.2014.978396
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发表时间：
2014-12-02
影响因子：
2.9
通讯作者：
Mahyudin, N. A.
中科院分区：
文献类型：
--
作者：
Yibadatihan, S.;Jinap, S.;Mahyudin, N. A.
棕榈仁饼（PKC）是家畜蛋白质和能量的重要来源。最近，它已被用作家禽饲料的成分。由于在生产和储存过程中处理不当而导致的PKC霉菌毒素污染增加了公众对家禽和人类经济损失和健康风险的关注。这一问题突出了PKC中真菌毒素评价的必要性。此外，迄今尚未建立用于定量PKC中真菌毒素的方法。因此，本研究的目的是（1）建立一种同时测定PKC中真菌毒素的方法，（2）验证和验证该方法。建立了电喷雾正、负离子液相色谱-串联质谱（LC-MS/MS）同时测定蛋白激酶C（PKC）中黄曲霉毒素（AFB（1）、AFB（2）、AFG（1）、AFG（2））、赭曲霉毒素A（OTA）、玉米赤霉烯酮（ZEA）、脱氧雪腐镰刀菌烯醇（DON）、伏马菌素（FB 1、FB 2）、T-2和HT-2毒素的方法。得到了最佳方法，即流速为0.2mlmin（-1），水相含0.2%甲酸，梯度开始时有机相含量为10%，梯度结束时有机相含量为90%。使用乙腈-水-甲酸（79：20：1，v/v）的溶剂混合物进行真菌毒素提取，无需进一步净化。加标PKC样本中真菌毒素的平均回收率范围为81%至112%。霉菌毒素标准品和蛋白激酶C样品的检出限（LOD）和定量限（LOQ）分别为0.02 - 17.5 μ g/kg和0.06 - 58.0 μ g/kg。最后，新开发的方法成功地应用于PKC样品。结果表明，该方法可同时测定PKC中多种霉菌毒素，可作为PKC常规分析的理想方法。
Palm kernel cake (PKC) is a useful source of protein and energy for livestock. Recently, it has been used as an ingredient in poultry feed. Mycotoxin contamination of PKC due to inappropriate handling during production and storage has increased public concern about economic losses and health risks for poultry and humans. This concern has accentuated the need for the evaluation of mycotoxins in PKC. Furthermore, a method for quantifying mycotoxins in PKC has so far not been established. The aims of this study were therefore (1) to develop a method for the simultaneous determination of mycotoxins in PKC and (2) to validate and verify the method. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using an electrospray ionisation interface (ESI) in both positive- and negative-ion modes was developed for the simultaneous determination of aflatoxins (AFB(1), AFB(2), AFG(1) and AFG(2)), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB1 and FB2), T-2 and HT-2 toxin in PKC. An optimum method using a 0.2mlmin(-1) flow rate, 0.2% formic acid in aqueous phase, 10% organic phase at the beginning and 90% organic phase at the end of the gradient was achieved. The extraction of mycotoxins was performed using a solvent mixture of acetonitrile-water-formic acid (79:20:1, v/v) without further clean-up. The mean recoveries of mycotoxins in spiked PKC samples ranged from 81% to 112%. Limits of detection (LODs) and limits of quantification (LOQs) for mycotoxin standards and PKC samples ranged from 0.02 to 17.5 mu gkg(-1) and from 0.06 to 58.0 mu gkg(-1), respectively. Finally, the newly developed method was successfully applied to PKC samples. The results illustrated the fact that the method is efficient and accurate for the simultaneous multi-mycotoxin determination in PKC, which can be ideal for routine analysis.