Validation and application of an analytical method for the determination of mycotoxins in crackers by UPLC-MS/MS

Abstract An analytical method applying ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was validated for the determination of aflatoxins M2, M1, G2, G1, B2, B1, deoxynivalenol, ochratoxin A, fumonisins B1 and B2, hydrolyzed fumonisins B1 and B2, zearalenone and sterigmatocystin in crackers. The obtained recoveries (70 to 110%) and relative standard deviations (< 13%) were considered satisfactory. Method limits of quantification ranged from 0.20 µg kg-1 (sterigmatocystin) to 12.27 µg kg-1 (deoxynivalenol). The validated method was then applied for mycotoxin determination in 60 cracker samples (cream crackers and water and salt crackers) obtained from the metropolitan area of the state of Rio de Janeiro, RJ. Deoxynivalenol, zearalenone and fumonisin B1 were found, respectively, in 100, 50 and 28% of the analyzed samples. The maximum permissible limits established by Brazilian legislation for deoxynivalenol and zearalenone were not exceeded in the analyzed samples.

摘要 本研究对一种采用超高效液相色谱-串联质谱法（ultra-performance liquid chromatography-tandem mass spectrometry，UPLC-MS/MS）的分析方法进行验证，以用于测定薄脆饼干中黄曲霉毒素M2、M1、G2、G1、B2、B1、脱氧雪腐镰刀菌烯醇（deoxynivalenol）、赭曲霉毒素A（ochratoxin A）、伏马菌素B1、伏马菌素B2、水解伏马菌素B1、水解伏马菌素B2（hydrolyzed fumonisins B1 and B2）、玉米赤霉烯酮（zearalenone）及柄曲霉素（sterigmatocystin）。实验所得回收率为70%~110%，相对标准偏差（RSD）小于13%，各项指标均令人满意。方法的定量限范围为0.20 μg·kg⁻¹（柄曲霉素）至12.27 μg·kg⁻¹（脱氧雪腐镰刀菌烯醇）。将验证后的方法应用于从巴西里约热内卢州都会区采集的60份薄脆饼干样品（包括奶油薄脆饼干与咸水薄脆饼干）的真菌毒素检测。在所检测的样品中，脱氧雪腐镰刀菌烯醇、玉米赤霉烯酮和伏马菌素B1的检出率分别为100%、50%和28%。所有受检样品中脱氧雪腐镰刀菌烯醇与玉米赤霉烯酮的含量均未超出巴西立法规定的最大允许限量。