SPE-HPLC-MS/MS测定粮食中玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇

Determination of Zearalenone and Deoxynivalenol in Cereal Grains by SPE-HPLC-MS / MS

建立了以乙腈-水（84：16，v／v）为提取溶剂、正己烷萃取和HLB固相萃取（SPE）净化、水和乙腈C18反相色谱梯度洗脱、电喷雾负离子多反应监测模式（MRM）同时测定粮食中玉米赤霉烯酮（ZEN）和脱氧雪腐镰刀菌烯醇（DON）2种物质含量的HPLC-MS／MS检测方法。结果表明，ZEN和DON检出限（以信噪比S／N：3计）依次为0．1μg/kg和2μg/kg，定量限（以信噪比S／N=10计）依次为0．3μg/kg和6μg／kg；两者线性范围分别为0．20～25μg／L（相关系数r=1．0000）和4．0～500μg／L（相关系数r=0．9999）；不同样品2种目标物3个水平的加标回收率在88．7％～102．3％之间，相对标准偏差（RSD）在2．4％～7．3％之间。应用该方法对所检小麦样品进行分析，结果均发现严重污染样品的2种目标毒素。

A method of SPE - HPLC - MS/MS was established for the content determination of ZEN and DON in cereal grains. The sample was extracted by acetonitrile -water （84： 16, v/v）, and then purified by the methods of solvent extraction and HLB solid phase extraction （SPE）. The chromatographic separation was performed on C18 column with gradient elution using acetonitrile and water as mobile phases, and the mass spectrometric acquisitions were carried out by means of multiple reaction monitoring （MRM） in electrospray negative ionization mode. The limits of detection （ LOD, S/N = 3） about ZEN and DON were 0.1 μg/kg and 2 μg/kg respectively, and the limits of quanti- fication （LOQ, S/N = 10） 0.3 μg/kg and 6 μg/kg respectively, and the ranges of linearity 0.20 - 25 μg/L（ r = 1. 000 0） and 4.0 - 500 μg/L （ r = 0. 999 9） respectively. The recoveries in different samples at three spiked concentration levels ranged from 88.7 % to 102.3 % with the relative standard deviations from 2.4 % to 7.3%.