摘要
采用同位素稀释法并结合凝胶色谱净化技术,建立了花生、粮油中18种常见真菌毒素污染的超高效液相色谱串联质谱分析方法。样品中添加同位素内标U—[13C17]-黄曲霉毒素B1和U-[13C15]-脱氧雪腐镰刀菌烯醇,经乙腈-水溶液(84:16,体积比)均质提取,凝胶渗透色谱净化,WatersACQUITYUPLCTMBEHC18色谱柱分离,串联四极杆质谱多反应离子监测方式检测,同位素稀释内标法定量。结果表明,18种真菌毒素在各自的线性范围内线性关系良好,相关系数均不低于0.996;其中12种化合物的定量下限为0.02.0.4μg-kg,6种负离子的定量下限为0.06~1.0μg/kg;低、中、高3个加标水平的回收率为80%~96%,相对标准偏差为10.5%~19.6%。该方法具有前处理简单、净化效果好、灵敏度高的优点,适用于复杂基质样品中多组分真菌毒素残留的确认和定量检测。
A method for the analysis of common mycotoxins in peanuts and oils was developed using ultra performance liquid chromatography with tandem mass spectrometry( UPLC -MS/MS), based on isotope dilution and gel permeation chromatography (GPC) purification. The homogenized sample was spiked with U - [ 13C17 ] - aflatoxin B1 and U - [ 13C15 ] - deoxynivalenol), and extracted with acetonitrile -water(84 : 16, by volume), then purified by GPC. The targeted compounds were detected by MS/MS system with eletrospray ionization(ESI) under muti-reaction monitoring(MRM) mode and quantified by the internal standard calibration curve of isotope dilution technique. The result indicated that the LOQ of 12 positive ions ranged from 0. 02μg/kg to 0.4μg/kg, the LOQ of 6 negative ions ranged from 0. 06μg/kg to 1.0 μg/kg. Meanwhile, the high correlation coefficents(r≥0. 996) of 18 mycotoxins were obtained within their respective linear ranges. The average recoveries at low, intermediate and high spiked levels ranged from 80% to 96% with relative standard deviations (RSD) of 10.. 5% - 19.6%. This method was suitable for the identification and quantification of multi-component mycotoxin contaminants in complex matrixes with advantages of simple pretreatment, good purification and high sensitivity.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第1期6-12,共7页
Journal of Instrumental Analysis
基金
山东检验检疫局科研基金资助项目(SK200822)
关键词
超高效液相色谱-串联质谱
凝胶渗透色谱
同位素内标
真菌毒素
ultra performance liquid chromatography -tandem mass spectrometry (UPLC -MS/ MS)
gel permeation chromatography(GPC)
isotope internal standard
mycotoxins