[关键词]
[摘要]
建立了超高效液相色谱-串联质谱法测定焙烤食品中4种链格孢菌毒素(腾毒素、链格孢菌酚、交链胞酚单甲醚、细交链胞菌酮酸)快速检测方法。样品经乙腈-0.1 mol/L盐酸溶液超声萃取,萃取液经QuEChERS净化处理,在RP18色谱柱(2.1 mm×100 mm,1.7 μm)上以乙腈和1 mmol/L碳酸氢铵为流动相梯度洗脱,采用电喷雾离子源、正负离子多反应监测模式检测,外标法定量。结果表明,4种待测物在相应的浓度范围内线性良好,相关系数均大于0.999;方法定量限(S/N≥10)为0.03~0.3 μg/kg;进行3个水平的添加回收实验,平均回收率(n=6)为83.2%~105.3%;相对标准偏差(RSD,n=6)为1.2%~6.4%。应用本方法检测45个焙烤食品样品,4种真菌毒素均有检出。其中24份样品检出AME,含量为0.1~4.6 μg/kg;6份样品检出AOH,含量为0.47~1.5 μg/kg;27份样品检出TeA,含量为0.6~3.7 μg/kg;9份样品检出TEN,含量为0.3~2.1 μg/kg。
[Key word]
[Abstract]
An analysis method using ultra-high performance liquid chromatography-tandem mass spectrometru (UPLC-MS/MS) was established for the determination of four alternaria toxins [Tenuazonic acid (TeA), Alternariol (AOH), Alternariol Monomethyl Ether (AME), Tentoxin (TEN)] in baked food. The samples were extracted with acetonitrile and 0.1 mol/L HCl, and the extracted solutions were purified using the QuEChERS approach. The target analytes were then separated on a RP18 column (2.1 mm×100 mm, 1.7 μm) using acetonitrile and 1 mmol/L NH4HCO3 as the mobile phase and detected by MS/MS under multiple reaction monitoring (MRM) mode. The mass spectrometry measurement was conducted using positive (ESI+) and negative (ESI-) electrospray ionization. Under the optimized conditions, the linearity of the four analytes were good in the corresponding concentration range with the correlation coefficients more than 0.999. The MLOQ was 0.03~0.3 μg/kg and the average recoveries (n=6) ranged from 83.2% to 105.3%, and relative standard deviation (RSD, n=6) in a range of 1.2%~6.4% when three levels of standard were spiked. This developed method was successfully applied for the detection of 45 baking food samples, and mycotoxins were detected in several samples. AME was detected in 24 samples with the concentrations ranged from 0.1 to 4.6 μg/kg; AOH was detected in 6 samples with the concentrations ranged from 0.47 to 1.5 μg/kg; TeA was detected in 27 samples with the concentrations ranged from 0.6 to 3.7 μg/kg; and TEN was detected in 9 samples with the concentrations ranged from 0.3 to 2.1 μg/kg.
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[基金项目]
广州市科技计划项目(201604020035)