固相萃取-超高效液相色谱-串联质谱法测定大米粉和小麦粉中白僵菌素和恩镰孢菌素  

Determination of beauvercin and enniatins in rice flour and wheat flour by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：赵迪 尹丹阳[1] 胡佳薇[1] 王敏娟[1] 刘宇[1] 乔海鸥[1] 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)

机构地区：[1]陕西省疾病预防控制中心,西安710054

出　　处：《卫生研究》2023年第5期756-761,768,共7页Journal of Hygiene Research

摘　　要：目的建立大米粉和小麦粉中白僵菌素、恩镰孢菌素A、恩镰孢菌素A1、恩镰孢菌素B、恩镰孢菌素B1的超高效液相色谱-串联质谱分析方法。方法样品用乙腈-水提取、Oasis Prime HLB固相萃取柱净化,Waters BEH C18色谱柱(2.1 mm×100 mm,1.8μm)分离,电喷雾电离正离子模式下多反应监测进行测定,同位素内标法和基质匹配标准曲线外标法定量。结果白僵菌素和4种恩镰孢菌素在0.1~50.0 ng/mL范围内具有良好的线性关系(r>0.999)。大米粉和小麦粉中白僵菌素和4种恩镰孢菌素的平均回收率分别是96.4%~105.4%和99.1%~109.2%,相对标准偏差分别为1.01%~7.42%和1.09%~9.69%(n=6),检出限为0.03μg/kg,定量限为0.1μg/kg,基质效应分别为72.7%~99.3%和60.8%~100.4%。面粉中白僵菌素和恩镰孢菌素污染水平高于大米,恩镰孢菌素B在小麦粉和大米粉中的检出率最高,含量分别为0.03~9.57μg/kg和0.03~0.56μg/kg,检出率分别为98.5%和36.4%。结论本方法简单快速、准确性好、灵敏度高,可用于小麦粉和大米粉中白僵菌素和恩镰孢菌素的测定。OBJECTIVE 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).METHODS 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,1.8μm).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.RESULTS The linear relationships of BEA and 4 kinds of enniatins(ENNs)were good in the range of 0.1-50.0 ng/mL(r0.999).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 0.03μg/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 0.03-9.57μg/kg and 0.03-0.56μg/kg,the positive percentage were 98.5%and 36.4%.CONCLUSION 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.

关 键 词：超高效液相色谱-串联质谱 白僵菌素 恩镰孢菌素 大米粉 小麦粉 

分 类 号：R155.54[医药卫生—营养与食品卫生学]