同位素内标-超高效液相色谱串联质谱法检测麦芽中11种真菌毒素

发布时间：2018-11-14 17:14

【摘要】：采用同位素内标法定量,建立了同时测定麦芽药材中11种真菌毒素污染水平的超高效液相色谱串联质谱法(UPLC-MS/MS)。采用乙腈-水-乙酸(80∶19∶1)溶剂系统超声提取药材中真菌毒素,离心、过滤后,加入[~(13)C_(17)]-AFB_1及[~(13)C_(18)]-ZEN标记的真菌毒素混合同位素标准溶液,以含0.1%甲酸的甲醇溶液-2 mmol·L~(-1)乙酸铵水溶液为流动相于Phenomenex Kinetex C_(18)色谱柱(100 mm×2.1 mm,2.6μm)上梯度洗脱分离,以电喷雾离子源正负离子切换模式多反应监测方式检测(MRM)。结果表明,11种真菌毒素在采用基质添加内标稳定同位素法定量时于各自的浓度范围内线性关系良好,r0.999 1,加标回收率为75.0%~117.0%,RSDs5.1%,检测限(LODs)和定量限(LOQs)分别为0.05~30μg·kg~(-1)和0.15~87.5μg·kg~(-1),远低于欧盟规定的真菌毒素最大允许残留量(MRLs)。所测的20批麦芽样品中,9批检测到真菌毒素残留,通过相同保留时间处的特征离子二级碎片排除了假阳性结果。该方法的样品前处理过程简便快捷、检测方法重现性好、灵敏度高,适用于复杂麦芽基质中多种真菌毒素的同时定性定量测定。
[Abstract]:An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of the contamination levels of 11 mycotoxins in Malt medicinal materials by isotopic internal standard method. The mycotoxins from medicinal materials were extracted by ultrasonic method using acetonitrile-water-acetic acid (80:19:1) solvent system. Adding [13C17]-AFB_1 and [13C18]-ZEN labeled mycotoxin mixed isotopic standard solution, The gradient elution separation was performed on a Phenomenex Kinetex C _ (18) column (100 mm 脳 2.1 mm,2.6 渭 m) with methanol solution containing 0.1% formic acid-2 mmol L ~ (-1) ammonium acetate as mobile phase. Detection of (MRM). By Multi-reaction Monitoring with positive and negative Ion switching Mode of Electrospray Ion Source The results showed that there was a good linear relationship between the concentration range of 11 mycotoxins and the stable isotopic method, r0.999 1, and the recovery rate was 75.0% and 117.0%, respectively. The detection limit (LODs) and the quantitative limit (LOQs) were 0.05U 30 渭 g kg~ (-1) and 0.15 渭 g kg~ (-1) respectively, which were far lower than the maximum allowable residue of mycotoxins (MRLs).) specified in the European Union. In the 20 batches of malt samples, 9 batches of mycotoxin residues were detected, and the false positive results were eliminated by the secondary fragments of characteristic ions at the same retention time. The method is simple, rapid, reproducible and sensitive. It is suitable for the simultaneous qualitative and quantitative determination of various mycotoxins in complex malt matrix.
【作者单位】：中国医学科学院北京协和医学院药用植物研究所;
【基金】：国家“重大新药创制”科技重大专项(2014ZX09304307-002) 国家自然科学基金面上项目(81274072,81473346) 协和新星人才支持计划
【分类号】：R284.1;O657.63

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