高效液相色谱-串联质谱法同时测定饲料中9种霉菌毒素及其代谢物  

Simultaneous Determination of Nine Kinds of Mycotoxins and Metabolins in Feed by High Performance Liquid Chromatography-tandem Mass Sepectrometry

作　　者：庄倩[1,2] 曲宝涵[1] 李彦 吴燕 穆阿丽 李辉 

机构地区：[1]青岛农业大学化学与药学院,山东青岛266109 [2]青岛市饲料兽药检测站,山东青岛266071

出　　处：《分析科学学报》2016年第1期37-42,共6页Journal of Analytical Science

基　　金：青岛市公共领域科技支撑计划(No.09-1-1-93-nsh)

摘　　要：应用高效液相色谱-串联质谱（HPLC-MS/MS）技术,建立了同时检测饲料中9种霉菌毒素及其代谢物的分析方法。样品加入NaCl经乙腈-水（85∶15）振荡提取后,用TC-M160多功能净化柱净化,氮气吹干,用1mL乙腈-水（1∶1）定容,Agilen C18色谱柱（150×2.1mm,3.5μm）分离,采用正负离子同时扫描的多反应监测模式进行检测,外标法定量。方法检出限为0.11~0.60μg/L,在2.0~100.0μg/L基质添加浓度范围内呈现良好的线性关系,相关系数r〉0.998。5.0~50.0μg/L加标范围内回收率为67.0%~103.5%,相对标准偏差〈15%。该法简便、快速、灵敏度高,符合对饲料中霉菌毒素的检测要求,可为相关检测提供技术支持。A method for the determination of nine mycotoxins and metabolins（aflatoxin B1（AFB1）,aflatoxin B2（AFB2）,aflatoxin G1（AFG1）,aflatoxin G2（AFG2）,T-2toxin,HT-2toxin,zearalenone（ZEN）,β-zearalenol（β-ZEL）,β-zearalanol（β-ZAL））in feed by high performance liquid chromatographytandem mass sepectrometry（HPLC-MS/MS）was developed.The samples were extracted with NaCl and acetonitrile-water（85∶15）using the mechanical shaking,then the solutions were purified by TC-M160multi-function purification column.The eluent was evaporated by nitrogen blow,dissolved in acetonitrilewater（1∶1）,separated by Agilent C18 chromatographic column（150×2.1mm,3.5μm）and the detection was used for multiple reaction monitoring which was operated both in positive and in negative ionization modes in chromatographic run.Quantification was done by external standard method.The limits of detection were 0.11-0.60μg/L,and the linear response was observed in the spiked concentration range of 2.0-100.0μg/L with the correlation coefficients higher than 0.998.At spiked levels of 5.0-50.0μg/L,the recoveries were 67.0%-103.5%,and the relative standard deviations were less than 15%.The method is a simple,fast,sensitive.and is complied with the regulations for the determination of mycotoxins in feed,and can provide more technical support for relevant determination.

关 键 词：霉菌毒素 饲料 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]