摘要
目的建立了玉米及其制品和小麦及其制品中白僵菌素(beauvericin,BEA)、恩镰孢菌素A(enniatin A,ENA)、恩镰孢菌素A_1(enniatin A_1,ENA_1)、恩镰孢菌素B(enniatin B,ENB)和恩镰孢菌素B_1(enniatin B_1,ENB_1)的高效液相色谱-串联质谱检测方法。方法样品经乙腈-水(85∶15,V/V)提取、室温静置、固相萃取柱净化后,以2 mmol/L乙酸铵水-乙腈作为流动相,采用电喷雾电离正离子多反应监测模式进行检测。结果该方法对玉米及其制品和小麦及其制品中BEA和4种恩镰孢菌素(ENNs)的检出限范围分别为0.01~0.12和0.02~0.21μg/kg,定量限范围分别为0.02~0.44和0.05~0.68μg/kg,平均加标回收率范围分别为91.6%~149.7%和100.5%~128.2%,基质抑制或增强效应分别为88.0%~101.5%和55.8%~106.5%,且BEA和4种ENNs在所测基质中线性关系和精密度良好,相关系数均>0.99,相对标准偏差均<15%。结论所建立的方法操作简便、灵敏度高、准确性好,可用于玉米及其制品和小麦及其制品中BEA和4种ENNs的测定。
Objective A high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS） for determination of beauvercin（ BEA）,enniatin A（ ENA）,enniatin A_1（ ENA_1）,enniatin B（ ENB） and enniatin B_1（ ENB_1） in corn,wheat and their products was developed. Methods Samples were extracted with acetonitrile-water（ 85 ∶ 15,V/V）,cleaned up with solid phase extraction column followed by HPLC-MS/MS determination with electrospray positive ionization（ ESI ＋） under multiple reaction monitoring（ MRM） mode,and with 2 mmol/L ammonium acetate water-acetonitrile as the mobile phase. Results The limits of detection for BEA and 4 kinds of enniatins（ ENNs） ranged from 0. 01 to 0. 12 μg/kg for corn and corn products and 0. 02 to 0. 21 μg/kg for wheat and wheat products,and the limits of quantification ranged from 0. 02 to 0. 44 μg/kg and 0. 05 to 0. 68 μg/kg for both cereals. The mean recoveries ranged from 91. 6 % to 149. 7 % for corn and corn products and 100. 5 % to 128. 2 % for wheat and wheat products,respectively.The matrix induced suppression or enhancement effect ranged from 88. 0 % to 101. 5 % and 55. 8 % to 106. 5 % for both cereals,respectively. The method for BEA and ENNs determination showed good linearity and precision in all matrixes with correlation coefficient above 0. 99,and the relative standard deviations were less than 15 %. Conclusion The method developed was of simple operation,high sensitivity and good accuracy,which could be used for BEA and 4 kinds of ENNs determination in corn and wheat and their products.
出处
《中国食品卫生杂志》
2017年第6期633-640,共8页
Chinese Journal of Food Hygiene
基金
科技基础工作专项(2013FY113400)
北京市自然科学基金(7163235)
关键词
玉米及其制品
小麦及其制品
高效液相色谱-串联质谱
白僵菌素
恩镰孢菌素
真菌毒素
食品污染物
Corn and their products
wheat and their products
high performance liquid chromatography-tandem massspectrometry
beauvercin
enniatins
mycotoxin
food contamination
