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采用液相色谱-串联质谱法(LC-MS/MS)同时测定棕榈仁饼(PKC)中的多种真菌毒素。

Simultaneous determination of multi-mycotoxins in palm kernel cake (PKC) using liquid chromatography-tandem mass spectrometry (LC-MS/MS).

机构信息

a Food Safety Research Centre (FOSREC), Faculty of Food Science and Technology , Universiti Putra Malaysia , Serdang , Malaysia.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2014;31(12):2071-9. doi: 10.1080/19440049.2014.978396. Epub 2014 Nov 17.

DOI:10.1080/19440049.2014.978396
PMID:25396715
Abstract

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 (AFB₁, AFB₂, AFG₁ and AFG₂), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB₁ and FB₂), T-2 and HT-2 toxin in PKC. An optimum method using a 0.2 ml min⁻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 μg kg⁻¹ and from 0.06 to 58.0 μg kg⁻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.

摘要

棕榈仁饼(PKC)是一种对牲畜具有高蛋白质和能量的有用来源。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,PKC 中的真菌毒素污染引起了人们对家禽和人类经济损失和健康风险的关注。这一关注突显了评估 PKC 中真菌毒素的必要性。此外,迄今为止,尚未建立 PKC 中真菌毒素的定量方法。因此,本研究的目的是:(1)建立同时测定 PKC 中真菌毒素的方法;(2)验证和验证该方法。建立了一种采用电喷雾离子化接口(ESI)在正离子和负离子模式下同时测定 PKC 中黄曲霉毒素(AFB₁、AFB₂、AFG₁和 AFG₂)、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(FB₁和 FB₂)、T-2 和 HT-2 毒素的液相色谱-串联质谱(LC-MS/MS)方法。采用 0.2 ml min⁻¹流速、水相 0.2%甲酸、起始 10%有机相和结束 90%有机相的梯度,实现了最佳方法。真菌毒素的提取采用乙腈-水-甲酸(79:20:1,v/v)溶剂混合物进行,无需进一步净化。真菌毒素在添加 PKC 样品中的平均回收率为 81%至 112%。真菌毒素标准和 PKC 样品的检测限(LOD)和定量限(LOQ)范围分别为 0.02 至 17.5 μg kg⁻¹和 0.06 至 58.0 μg kg⁻¹。最后,成功地将新开发的方法应用于 PKC 样品。结果表明,该方法对于 PKC 中多种真菌毒素的同时测定是高效和准确的,可用于常规分析。

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