Zhao Di, Yin Danyang, Hu Jiawei, Wang Minjuan, Liu Yu, Qiao Haiou
Center for Disease Control and Prevention of Shaanxi Province, Xi'an 710054, China.
Wei Sheng Yan Jiu. 2023 Sep;52(5):756-768. doi: 10.19813/j.cnki.weishengyanjiu.2023.05.011.
To develop a method for the determination of beauvercin(BEA), enniatin A(ENNA), enniatin A1(ENNA1), enniatin B(ENNB) and enniatin B1(ENNB1) in rice flour and wheat flour by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).
Samples were extracted by acetonitrile-water, purified by Oasis Prime HLB solid-phase extraction column. The sample solution was separated by waters BEH C_(18) column(2.1 mm×100 mm, 1.8 μm). The detection was performed in the electrospray positive ionization(ESI+) under multiple reaction monitoring(MRM) mode. The internal standard method and the matrix-matched calibrations were used for quantification.
The linear relationships of BEA and 4 kinds of enniatins(ENNs) were good in the range of 0.1-50.0 ng/mL(r>0.999). The average recoveries of BEA and ENNs in rice flour and wheat flour were 96.4%-105.4% and 99.1%-109.2%, with the relative standard deviations(RSD) of 1.01%-7.42% and 1.09%-9.69%(n=6). The detection limits(LOD) of BEA and ENNs were 0.03 μg/kg. The quantitative limits(LOQ) of BEA and ENNs were 0.1μg/kg. The matrix induced suppression or enhancement effect were 72.7%-99.3% and 60.8%-100.4%, respectively. The levels of emerging BEA and ENNs in wheat flour were higher than rice flour. The detection rate of enniatin B was highest in wheat flour and rice flour, the contents were 0.03-9.57 μg/kg and 0.03-0.56 μg/kg, the positive percentage were 98.5% and 36.4%.
The method is quick, easy, accurate and sensitive, which is suitable for the determination of BEA and 4 kinds of ENNs in rice flour and wheat flour.
建立超高效液相色谱 - 串联质谱法（UPLC - MS/MS）测定米粉和面粉中白僵菌素（BEA）、恩镰孢菌素A（ENNA）、恩镰孢菌素A1（ENNA1）、恩镰孢菌素B（ENNB）和恩镰孢菌素B1（ENNB1）的方法。
样品用乙腈 - 水提取，经Oasis Prime HLB固相萃取柱净化。样品溶液采用waters BEH C₁₈柱（2.1 mm×100 mm，1.8 μm）分离。在电喷雾正离子化（ESI +）模式下，采用多反应监测（MRM）进行检测。采用内标法和基质匹配校准进行定量。
BEA和4种恩镰孢菌素（ENNs）在0.1 - 50.0 ng/mL范围内线性关系良好（r＞0.999）。米粉和面粉中BEA和ENNs的平均回收率分别为96.4% - 105.4%和99.1% - 109.2%，相对标准偏差（RSD）分别为1.01% - 7.42%和1.09% - 9.69%（n = 6）。BEA和ENNs的检测限（LOD）为0.03 μg/kg。BEA和ENNs的定量限（LOQ）为0.1 μg/kg。基质诱导抑制或增强效应分别为72.7% - 99.3%和60.8% - 100.4%。面粉中新兴BEA和ENNs的含量高于米粉。面粉和米粉中恩镰孢菌素B的检出率最高，含量分别为0.03 - 9.57 μg/kg和0.03 - 0.56 μg/kg，阳性率分别为98.5%和36.4%。
该方法快速、简便、准确、灵敏，适用于米粉和面粉中BEA和4种ENNs的测定。
