中文摘要：建立了谷物及其制品中脱氧雪腐镰刀菌烯醇、3-乙酰脱氧雪腐镰刀菌烯醇、15-乙酰脱氧雪腐镰刀菌烯醇、去环氧脱氧雪腐镰刀菌烯醇的同位素稀释-超高效液相色谱-线性离子阱串联质谱(UHPLC-QTRAP-MS/MS)定性确证和定量测定方法。样品经乙腈-水(84∶16,V/V)混合溶液提取,乙腈饱和的正己烷除脂,HLB固相萃取柱净化,Waters Atlantis~T3色谱柱分离,以乙腈-0.02%氨水溶液为流动相进行梯度洗脱,在负离子模式下,采用多反应监测(MRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,在线EPI谱库定性分析,同位素内标定量,在1~300μg/L浓度范围内,4种目标物的线性相关系数均大于0.999,检出限为0.1μg/kg,定量限为0.3μg/kg,添加5,50和200μg/kg的3个浓度水平,4种目标物的平均回收率均在81.3%~101.7%之间,相对标准偏差均小于5%,将该技术应用于FAPAS阳性玉米质控样品和5种代表性的样品进行测试,结果表明,本方法简单、准确、快速,适用于谷物及其制品中呕吐毒素及其衍生物和代谢物的快速确证和定量测定。
外文摘要：A method was established for the qualitative identification and quantitative determination of DON,3-Ac-DON,15-Ac-DON,DOM-1 in cereal and cereal products based on solid phase extraction and ultra performance liquid chromatography-quadrupole linear ion trap mass spectrometry(UPLC-QTRAP-MS / MS)with isotopic dilution. Samples were extracted by the mixture of acetonitrile and water(84 ∶ 16,V / V),degreased by hexane saturated with acetonitrile and purified by HLB solid phase extraction cartridge. The target analytes were separated by Waters Atlantis~ T3 column with gradient elution by mobile phases which consisted of acetonitrile and 0. 02% ammonia water. A scheduled multiple reaction monitoring(MRM)in negative mode as survey scan and an enhanced product ion(EPI)scan as dependent scan in an information dependent acquisition(IDA)experiment were adopted in mass spectrometry acquisition. On-line lab-built MS / MS library as well as the isotope internal standards was employed for the identification and qualification.For each analyte,the correlation coefficient was above 0. 999 in the linear range of 1-300 μg / L. The limits of detection(LOD)and quantitation(LOQ)were 0. 1 μg / kg and 0. 3 μg / kg,respectively. The mean recovery was 81. 3%-101. 7% at three spiked levels of 5,50,200 μg / kg. The relative standard deviation(RSD)was no more than 5%. The proposed method was successfully applied to the analysis of FAPAS′s QC samples and five representative samples. This method was simple,fast and precise,and suitable for the determination and confirmation of deoxynivalenol and its derivatives and metabolites in cereal and cereal products.
外文关键词：Isotopic dilution；Deoxynivalenol and its derivatives and metabolites；Ultra performance liquid chromatography；Quadrupole linear ion trap mass spectrometry
作者：Liu, Z；Hua, Y；Xu, XY；Chen, WQ；Zhao, CQ；Liang, JJ；Ding, YQ；Luo, JW
作者单位：Zhejiang Inst Food & Drug Control
期刊名称：CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
期刊影响因子：0.554
出版年份：2016
出版刊次：11
点击下载：同位素稀释－超高效液相色谱－线性离子阱串联质谱分析谷物及其制品中呕吐毒素及其衍生物和代谢物