本文旨在建立利用超高效液相色谱-串联质谱(Ultra Performance Liquid Chromatogra-phy Tandem Mass Spectrometry,UPLC-MS/MS)同时测定糙米、稻壳和秸秆样品中的氟酮磺草胺及其代谢物BCS AA10030和BCS-CS64946。样品经乙腈水溶液振荡提取,PSA、C18或GCB净化,UPLC-MS/MS测定,外标法定量。氟酮磺草胺、BCS AA10030 和BCS-CS64946 在0。001~0。5 mg/L范围内线性关系较好,相关系数>0。997 0,检出限均为0。01 mg/kg,在0。01、0。05、0。1三个添加水平下,氟酮磺草胺及其代谢物BCS AA10030和BCS-CS64946在糙米、稻壳和秸秆中平均回收率均分别为88。4%~103。0%,相对标准偏差分别为0。9%~9。3%,3种化合物在糙米、稻壳和秸秆中的定量限均为0。01 mg/kg,。该方法能够满足水稻中氟酮磺草胺及其代谢物残留分析要求,适用于大量水稻样品中氟酮磺草胺及其代谢物的快速检测,为政府监管提供有效的检测分析手段。
Simultaneous Determination of Residues of Triafamone and Its Metabolites in Rice by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
This study aims to establish a method for the determination of triafamone and its metabolites BCS AA10030 and BCS-CS64946 in brown rice,rice husk and straw samples by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC MS/MS).The samples were extracted by acetonitrile solution,purified by PSA,C18 or GCB,and analyzed by UPLC-MS/MS.Quantification was performed using external standard method.The linear relationships between triafamone,BCS AA10030 and BCS-CS64946 were found to be highly dependent in the range of 0.001~0.5mg/L,with correlation coefficient greater than 0.997 0.The average recoveries of triafamone and its metabolites BCS AA10030 and BCS-CS64946 in brown rice,rice husk and straw ranged from 88.4%to 103.0%at three spiked concentration levels of 0.01,0.05 and 0.1 mg/kg,with relative standard deviations of 0.9%~9.3%,respectively.The limits of quantitation for the three compounds in brown rice,rice husk and straw were determined to be 0.01 mg/kg.The method meets the requirements for residue analysis of triafamone and its metabolites in rice and is suitable for rapid detection in a large number of rice samples,providing an effective means of detection and analysis for government supervision.
triafamonemetabolitesultra performance liquid chromatography tandem mass spec-trometry(UPLC-MS/MS)rice