中心切割二维液相色谱串联质谱法分析烟草农残研究  

Analysis of Pesticide Residues in Tobacco Using Heart-cutting Two Dimensional Liquid Chromatography-tandem Mass Spectrometry

作　　者：陈敏[1,2] 王轩堂[1] 吴达 戚大伟[2] 罗辰[2] 刘百战[2] 张祥民[1] CHEN Min;WANG Xuantang;WU Da;QI Dawei;LUO Chen;LIU Baizhan;ZHANG Xiangmin(Fudan University, Shanghai 200433, China;Shanghai Tobacco Group Co., Ltd., Shanghai 200082, China)

机构地区：[1]复旦大学,上海200433 [2]上海烟草集团有限责任公司技术中心,上海200082

出　　处：《中国烟草科学》2017年第6期41-47,共7页Chinese Tobacco Science

摘　　要：开发了中心切割二维液相色谱/串联质谱联用分析烟草多种农药残留的技术。该方法采用二维液相色谱串联质谱,第一维体积排阻色谱与第二维反相液相色谱通过定量环进行转移。第一维的体积排阻色谱分离去除大分子物质,目标馏分经分流后切割至六通阀上的定量环。目标物收集完成时通过阀转动第二维流动相将目标物带入第二维反相液相色谱进一步分离。运用质谱的多反应监测模式(multi reaction monitoring,MRM)对74种农残进行定性定量分析,检测结果与一维LC-MS/MS方法较为一致,农药回收率72%~136%,定量限0.022~0.152 mg/kg。研究开发的中心切割多维液相色谱/串联质谱联用测定烟草农残方法可由仪器自动运行,结果准确可靠,适合于大量烟草样品多组分农残的自动分析检测。A new concept for sample cleanup,based on size exclusion of macro molecular compounds in matrix,has been developed by coupling of gel permation chromatography(GPC)with LC-MS/MS.Heart-cutting two-dimensional liquid chromatography tandem mass spectrometry system was used by transferring the target elution through a loop.In the two dimensional liquid chromatography-tandem mass spectrometry system,a GPC column was employed in the first dimension to separate the macromolecule interference compound weight.After split,the target fluent were heart-cutting to a loop connected to a6-way valve.Then the valve switched,so the second dimensional mobile phase took the target compounds for further reversed phase liquid chromatographic separation.Finally,about80different species of pesticide residues were determined qualitatively and quantitatively under the multi reaction monitoring(MRM)mode.The recoveries of most pesticides were in the range of72%-136%and the limits of quantitation(LODs)for this method were from0.022to0.152mg/kg.Compared to conventional approaches for pesticide residue analysis in tobacco,the new technique involves less contamination of ion source in MS without sacrificing method LODs.In addition,the2DLC-MS/MS method was fully automatic and the results were also accurate when utilized to detection of tobacco samples.

关 键 词：农残 烟草 二维液相色谱 中心切割 

分 类 号：O657.63[理学—分析化学] S481.8[理学—化学]