QuEChERS-SPE-超高效液相色谱-串联质谱法测定调味面制品中的12种真菌毒素

建立了QuEChERS-SPE-超高效液相色谱-串联质谱法检测调味面制品中12种真菌毒素残留量的方法.样品由甲酸-乙腈-水溶液提取,加入氯化钠和无水硫酸镁盐析分层,取部分上层清液经Prime HLB小柱萃取净化,净化后的液体再加入无水硫酸镁、乙二胺-N-丙基硅烷(PSA)、C18和中性氧化铝粉末(Al-N)净化;以Wa...

Determination of 12 Mycotoxins in Seasoning Flour Products by QuEChERS-SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method was developed for the residual quantity determination of 12 mycotoxins in seasoning flour products by QuEChERS-SPE-ultra performance liquid chromatography-tandem mass spectrometry. The samples were extracted with formic acid acetonitrile aqueous solution and salted out by adding sodium chloride and anhydrous magnesium sulfate. The supernatant was taken and purified by Prime HLB column extraction. The purified liquid was further cleaned up by adding anhydrous magnesium sulfate, PSA, C₁₈ and Al-N. The target compound, which was separated with Waters CORTECS C₁₈+ column, was eluted by gradient elution. The electrospray ion source (ESI) positive ion mode and multiple reaction monitoring mode (MRM) were used for mass spectrometry. Take negative samples as ground substance whitespace along with matching standard curve. The quantification was achieved by external standard method. The results showed that within the scope of 0.3~1000 ng/mL, the linear relationships of 12 mycotoxins were very good, the determination coefficient (R2) of which were higher than 0.99. The limits of detection were 0.10~3.0 μg/kg, and the limits of quantity were 0.30~10.0 μg/kg. Under the adding levels of high and medium as well as low, the average adding standard recoveries of 12 mycotoxins were 84.2%~97.2% and the relative standard deviations (RSDs) were 3.25%~8.77% (n=6). This method with high recovery rate and high sensitivity was rapid and accurate, which would be used to simultaneously determinate the 12 mycotoxins in seasoning flour products.