摘要
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)、C_(18)和中性氧化铝粉末(Al-N)净化;以Waters CORTECS C_(18)+色谱柱分离,梯度洗脱目标化合物,质谱分析采用电喷雾离子源(ESI)正离子模式和多反应监测方式(MRM),以阴性样品为基质空白,匹配标准曲线,外标法定量。研究结果:在浓度0.3~1000 ng/mL范围内,此12种真菌毒素线性关系良好,决定系数(R^(2))大于0.99,方法检出限为0.10~3.0μg/kg,定量限为0.30~10.0μg/kg;取低、中、高三个添加水平下,12种真菌毒素的平均加标回收率为84.2%~97.2%,相对标准偏差为3.25%~8.77%(n=6)。该方法具有回收率高、准确、快速、灵敏度高等特点,可同时对调味面制品中12种真菌毒素残留量进行测定。
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,C_(18) and Al-N.The target compound,which was separated with Waters CORTECS C_(18)+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(R^(2))of which were higher than 0.99.The limits of detection were 0.10~3.0μg/kg,and the limits of quantity were 0.30~10.0μg/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.
作者
徐子婷
郝莉花
马静
卫润鑫
李晓明
范雯婷
路书彦
XU Ziting;HAO Lihua;MA Jing;WEI Runxin;LI Xiaoming;FAN Wenting;LU Shuyan(Henan Product Quality Supervision and Inspection Institute,Zhengzhou 450000,China)
出处
《食品工业科技》
CAS
北大核心
2022年第6期311-319,共9页
Science and Technology of Food Industry
基金
河南省市场监督管理局科技计划项目(2020sj19)
河南省重点研发与推广专项(科技攻关)项目(212102410005)。
关键词
超高效液相色谱-串联质谱
QUECHERS
固相萃取
调味面制品
真菌毒素
ultra performance liquid chromatography-tandem mass spectrometry
QuEChERS
solid phase extraction
seasoning flour products
mycotoxins
