分析测试学报2025，Vol.44Issue(11)：2354-2361,8.DOI:10.12452/j.fxcsxb.250222112
高效液相色谱-串联质谱法同时测定粮谷中13种真菌毒素
Simultaneous Determination of 13 Mycotoxins in Grains by High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)analytical method was developed for the determination of thirteen mycotoxins in grains by using Capti-va EMR-Lipid column for purification.After being grinded,samples were extracted with acetoni-trile-water-formic acid(84∶15∶1,volume ratio).Extract solution was purified by Captiva EMR-Lipid solid phase extraction column,and then concentrated by nitrogen blowing,diluted to a certain volume and determined.The targets were seperated on a XSelect HSS T3(2.1 mm×100 mm,3.5μm)column.Acetonitrile and 0.1％formic acid water were selected for the positive ion mode and methanol and 0.1％ammonia water for the negative mode.Gradient elution and mass spectrometry un-der multiple reaction monitoring(MRM)mode were used for testing and external standard method was used for quantitative analysis.Thirteen mycotoxins exhibited good linear relationships across different mass concentration ranges with their correlation coefficients(r2)greater than 0.99.The limits of de-tection(LOD)were 0.10-3.12 μg/kg,and limits of quantitation(LOQ)were 0.33-10.4 μg/kg.Corn,wheat,rice,and sorghum were used as the blank matrix,and spiked at three levels of high,medium,and low.The average recoveries were 76.4％-108％,and the relative standard deviations(RSDs)were 3.2％-8.8％(n=6).Imported grain samples were tested by the method.Aflatoxin B1,T-2 and ochratoxin A were detected in a rice sample,and zearalanone was detected in a corn sam-ple.The method is accurate,reliable and reproducible,which can be used for the quantitative anal-ysis of thirteen mycotoxins for imported grains.关键词
高效液相色谱-串联质谱(HPLC-MS/MS)/真菌毒素/粮谷/同时测定Key words
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/mycotoxin/grains/simultaneous determination分类
化学引用本文复制引用
孙良娟,郑羽茜,唐媛媛,李红权,冯祥龙,庞田润..高效液相色谱-串联质谱法同时测定粮谷中13种真菌毒素[J].分析测试学报,2025,44(11):2354-2361,8.基金项目
海关总署科研项目(2021HK205) （2021HK205）
湛江海关科研项目(2024ZJHK005) （2024ZJHK005）
湛江市科技项目(2024B01084) （2024B01084）
