Hu Qiaoru, Cao Peng, Cong Zhongxiao, Liang Junni, Sha Meilan, Li Xiaoyu, Yin Dalu, Lu Min
Yantai Customs Technology Center, Yantai 264000, China.
Se Pu. 2019 Nov 8;37(11):1241-1248. doi: 10.3724/SP.J.1123.2019.03041.
A rapid method based on ultrahigh-performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-HRMS) was developed for the screening and confirmation of 20 mycotoxins in grain products. The samples were extracted with acetonitrile containing 2% (v/v) formic acid, and the extracts were cleaned up on Captive EMR-Lipid columns. The analytes were separated on a Thermo Hypersil Gold C column (100 mm×2.1 mm, 1.9 μm), and analyzed by UPLC-HRMS. The retention time and accurate mass of the parent ion were used for fast screening in full scan mode, while the accurate masses of the fragment ions were used for confirmation in the two-stage threshold-triggered full mass scan mode. The results revealed that the 20 mycotoxins showed good linear relationships in their respective mass concentration ranges. The correlation coefficients were not less than 0.99, and the limits of quantitation (LOQs) ranged from 0.25 to 20 μg/kg. The recoveries of the 20 mycotoxins in the sample ranged from 72.9% to 117.8% with the relative standard deviations (RSDs) from 2.9% to 15.2% at three spiked levels (=6). This method has the advantages of high sensitivity and reliability, and is thus suitable for the rapid screening and confirmation of 20 mycotoxins in grain products.
建立了一种基于超高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法(UPLC-HRMS)的快速方法,用于谷物产品中20种霉菌毒素的筛查和确证。样品用含2%(v/v)甲酸的乙腈提取,提取物在Captive EMR-Lipid柱上进行净化。分析物在Thermo Hypersil Gold C柱(100 mm×2.1 mm,1.9 μm)上分离,并用UPLC-HRMS进行分析。母离子的保留时间和精确质量用于全扫描模式下的快速筛查,而碎片离子的精确质量用于两级阈值触发全质量扫描模式下的确证。结果表明,20种霉菌毒素在各自的质量浓度范围内呈现良好的线性关系。相关系数不小于0.99,定量限(LOQs)范围为0.25至20 μg/kg。样品中20种霉菌毒素在三个加标水平(n = 6)下的回收率为72.9%至117.8%,相对标准偏差(RSDs)为2.9%至15.2%。该方法具有灵敏度高、可靠性强的优点,适用于谷物产品中20种霉菌毒素的快速筛查和确证。