PRIME-HLB固相萃取/超高效液相色谱-串联质谱法同时快速检测粮食中4种真菌毒素的含量

Simultaneous Determination of 4 Mycotoxins in Grains by UPLC-MS/MS Coupled with PRIME-HLB SPE Clean-up

建立了超高效液相色谱-三重四级杆串联质谱法同时快速检测粮食中呕吐毒素、赭曲霉毒素A、玉米赤霉烯酮和黄曲霉毒素B1的方法.样品经乙腈-水混合液(体积比84∶16)振荡提取20 min,乙腈饱和正己烷除脂,经PRIME-HLB小柱净化,氮吹浓缩后定容.质谱采用电喷雾正、负离子模式并选择多反应监测方式采集数据,外标法定量.方法的定量限(3S/N):呕吐毒素20.0μg/kg、赭曲霉毒素A 1.0μg/kg、玉米赤霉烯酮5.0μg/kg及黄曲霉毒素B10.2μg/kg.用该方法检测小麦、玉米、大米和高粱等试样,4种真菌毒素的加标回收率介于75.5%~98.6%之间,相对标准偏差不大于6.6%(n=6).

A method was developed for the simultaneous rapid determination of 4 mycotoxins such as deoxynivalenol,ochratoxin A,zearalenone,aflatoxins B1 in grains by PRIME-HLB solid-phase extraction/ultra high performance liquid chromatography tandem mass spectrometry.Samples were firstly extracted with acetonitrile-water(84∶16,v/v) for 20 min and defatted with acetonitrile-saturated n-hexane,then purified by PRMIE HLB column,and eluent was finally concentrated by nitrogen and diluted to volume and filtrated.The target drug residues were determined by multiple reaction monitoring mode by positive and negative electrospray ionization,and quantified by the method of external standard.The limits o f detection(S/N=3) were separately 20.0 μg/kg for deoxynivalenol,1.0 μg/kg for ochratoxin A,5.0 μg/kg for zearalenone and 0.2 μg/kg for aflatoxins B1.The proposed method was applied to the analysis of samples of grains residues,giving the accuracy of in the range of 75.5%~98.6%,with RSD less than 6.6%(n=6).