固相支撑液液萃取/超高效液相色谱-串联质谱法测定牧草中真菌毒素  

Determination of Mycotoxins in Forage Grass by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Solid Supported Liquid-Liquid Extraction

作　　者：韩祎陟 盛万里 王晓敏 任彩霞 张春艳 郑书展 HAN Yi-zhi;SHENG Wan-li;WANG Xiao-min;REN Cai-xia;ZHANG Chun-yan;ZHENG Shu-zhan(Technical Center of Hohhot Customs,Hohhot 010020,China)

机构地区：[1]呼和浩特海关技术中心,内蒙古呼和浩特010020

出　　处：《分析测试学报》2025年第3期506-513,共8页Journal of Instrumental Analysis

基　　金：海关总署科研项目(2022HK122,2023HK082)。

摘　　要：建立了基于固相支撑液液萃取和超高效液相色谱-串联质谱技术的牧草中11种常见真菌毒素的快速检测方法。在优化的色谱条件下,实现了两对同分异构体(β-玉米赤霉醇和α-玉米赤霉醇,β-玉米赤霉烯醇和α-玉米赤霉烯醇)的色谱分离。牧草样品选择含1%甲酸的乙腈/水(体积比8∶2)为提取溶剂,固相支撑液液萃取法上柱萃取前每毫升提取液加入3.0 mL水,使用乙酸乙酯为洗脱液,结果显示净化效果明显,基质效应较弱。在常见的苜蓿、燕麦、羊草、青贮玉米中验证了方法适用性,11种真菌毒素在各自线性范围内线性关系良好(r^(2)>0.995),检出限为0.3~20.3μg/kg,定量下限为0.8~51.4μg/kg,方法的平均回收率为72.7%~108%,相对标准偏差(RSD)为3.4%~8.1%。该方法稳定可靠、操作简便、成本低廉,定量下限满足国内外相关监管限量要求,适用于牧草中多种真菌毒素的同步筛查和确证检测。A new method for the simultaneous determination of 11 mycotoxins(aflatoxin B_(1),aflatoxin B_(2),aflatoxin G_(1),aflatoxin G_(2),zearalenone,zearalanone,β-zearalanol,α-zearalanol,β-zearalenol,α-zearalenol and deoxynivalenol)in forage grass by means of solid supported liquid-liquid extraction(SLE)coupled with ultra high performance liquid chromatography-tandem mass spectrometry has been established.In this study,two pairs of mycotoxins epimers(β-zearalanol andα-zearalanol,β-zearalenol andα-zearalenol)were separated completely under optimized chromatographic conditions.The sample were extracted with 1%formic acid acetonitrile/water(8∶2),and then purified by a diatomaceous earth SLE cartridge.Series of experiment conditions such as the extraction solvent type and the volume of elution solvent was examined and optimized,6 mL ethyl acetate was the suitable elution solution.The matrix effects of mycotoxins in alfalfa,oats,leymus chinensis and silage corn were discussed,and the interference of matrix was reduced by the matrix matched calibration standards curve.Results showed good linearity(r^(2)>0.995)for determination of 11 mycotoxins.The limits of detection(LODs)and the limits of quantitation(LOQs)were in the ranges of 0.3μg/kg to 20.3μg/kg and 0.8μg/kg to 51.4μg/kg,respectively.Recoveries for 11 mycotoxins at three spiked levels ranged from 72.7% to 108%with relative standard deviations(RSDs)ranged from 3.4%to 8.1%.The method has the advantages of simple operation,good reproducibility and accurate,and the LOQ of method were lower than the specific migration limit specified in the regulation and standards.The proposed method has great potentials in the detection of mycotoxins in forage grass.

关 键 词：真菌毒素 牧草 固相支撑液液萃取 超高效液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]