摘要
采用液相色谱-串联质谱建立了小麦中T-2、玉米赤霉烯酮(ZEN)和脱氧镰刀菌烯醇(DON)的测定方法。样品经80%乙腈-水提取,氨基柱(500 mg,6 mL)杂质吸附模式净化,以5 mmol/L乙酸铵溶液和甲醇为流动相,ZORBAX Extend-C18柱(150 mm×2.1 mm,1.8μm)进行色谱分离;在电喷雾正离子化模式下,多反应监测方式测定。结果表明:T-2、ZEN和DON分别在0.5~500、5~500、10~2 000μg/L质量浓度范围内呈良好线性,相关系数分别为0.998 9、0.999 7和0.999 1。通过对空白小麦样品进行3个水平的加标回收实验,T-2、ZEN和DON的回收率分别为86%~94%、80%~101%和81%~105%,相对标准偏差(RSD)分别为2.6%~5.5%、3.6%~8.9%和2.2%~8.1%,方法检出限分别为0.5、8.0、10.0μg/kg。该方法准确、灵敏、成本低,适用于小麦中T-2、ZEN和DON的同时分析。
A liquid chromatography tandem mass spectrometric(LC-MS/MS)method was developed for the simultaneous determination of T-2,zearalenone(ZEN) and deoxynivalenol(DON) in wheat.The sample was extracted with acetonitrile-water(80 ∶ 20).The extract was purified with an Amino column(AccuBond AMINO,500 mg,6 mL).Three myctoxins were completely separated on a ZORBAX Extend-C18 column(150 mm×2.1 mm,1.8 μm)by gradient elution with methanol and 5 mmol/L ammonium acetate as mobile phase,and detected by positive ion electrospray ionization mass spectrometry(ESI MS) under multiple reaction monitoring(MRM) mode.The results showed that the linearities of T-2,ZEN and DON were in the concentration ranges of 0.5-500,5-500,10-2 000 μg/L,respectively,with correlation coefficients of 0.998 9,0.999 7 and 0.999 1,respectively.The spiked recoveries of T-2,ZEN and DON at three spiked levels in wheat were in the ranges of 86%-94%,80%-101% and 81%-105%,with relative standard deviations(RSDs,n=5) of 2.6%-5.5%,3.6%-8.9% and 2.2%-8.1%,respectively.The limits of detection for T-2,ZEN and DON were 0.5,8.0,10.0 μg/kg,respectively.The method was low cost,sensitive and accurate,and was suitable for the simultaneous determination of T-2,ZEN and DON in wheat.
出处
《分析测试学报》
CAS
CSCD
北大核心
2012年第2期169-173,共5页
Journal of Instrumental Analysis
基金
中央级公益性科研院所基本科研业务费专项资金资助项目(2009RG006)
关键词
固相萃取柱
液相色谱-串联质谱
真菌毒素
小麦
solid phase extraction(SPE)
liquid chromatography-tandem mass spectrometry(LC-MS/MS)
mycotoxins
wheat