超高效合相色谱-串联质谱手性分离和测定烟草及土壤中茚虫威对映体  

Enantioseparation and determination of indoxacarb in tobacco and soil by ultra-performance convergence chromatography with tandem mass spectrometry

作　　者：杨飞[1] 李中皓[1] 王颖[1] 刘珊珊[1] 范子彦[1] 边照阳[1] 唐纲岭[1] 邓惠敏[1] YANG Fei;LI Zhonghao;WANG Ying;LIU Shanshan;FAN Ziyan;BIAN Zhaoyang;TANG Gangling;DENG Huimin(China National Tobacco Quality Supervision & Test Center,Zhengzhou 450001,China)

机构地区：[1]国家烟草质量监督检验中心

出　　处：《烟草科技》2019年第7期75-82,共8页Tobacco Science & Technology

摘　　要：为实现烟草和土壤中茚虫威对映体的手性分离和测定,建立了超高效合相色谱-串联质谱(UPC^2-MS/MS)快速分离和测定烟草及其土壤中茚虫威对映体的方法。样品经QuEChERS方法处理后,以CO2和甲醇为流动相,用Chiralcel IG-3色谱柱分离样品,并在多反应监测模式(MRM)下进行MS/MS分析,采用基质匹配标准工作曲线法定量。结果表明:①该方法实现了R-/S-茚虫威对映体的基线分离,手性分离时间仅为5min。②在对映体含量为2.5、7.5和15.0mg/kg水平下,各对映体的回收率为83.7%~96.6%,日间相对标准偏差(RSD)<6.0%。在质量浓度50~1000ng/mL范围内,烟草和土壤基质中两种对映体的线性良好(R^2≥0.9932)。两种基质中对映体的检出限(LOD)和定量限(LOQ)分别为0.028~0.048和0.088~0.148mg/kg。③采用该方法对10个烟叶和10个土壤实际样品进行了检测,仅有1个土壤样品检出R-茚虫威(1.05mg/kg)和S-茚虫威(0.88mg/kg)。该方法绿色、快速、可靠,适用于烟草及其土壤中茚虫威对映体的分离和测定。In order to enantioseparate and analyze the indoxacarb in tobacco and soil, a method was proposed for the simultaneous enantiomeric analysis of indoxacarb in tobacco and soil using ultra-performance convergence chromatography with tandem mass spectrometry (UPC^2-MS/MS). Sample preparation prior to UPC^2-MS/MS analysis followed QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure. The UPC2-MS/MS method used a Chiralcel IG-3 column with a mobile phase consisting of CO2 and methanol. The extract was analyzed quantitatively by UPC2-MS/MS under the multiple reaction monitoring (MRM) mode, and the results were quantified by matrix matching standard working curve. The results showed that: 1) The enantiomer of indoxacarb reached baseline separation, and the chiral separation time was only 5 minutes. 2) Under the optimal conditions, the recoveries for the enantiomers were 83.7%-96.6% with relative standard deviation (RSD) less than 6.0% at 2.5, 7.5 and 15.0 mg/kg levels. Good coefficients of determination (R^2≥0.993 2) were achieved for all studied enantiomers in the tobacco and soil in the concentration range of 50-1 000 ng/mL. The LOD for the enantiomers in tobacco and soil varied from 0.028 to 0.048 mg/kg, and the LOQ varied from 0.088 to 0.148 mg/kg. 3) Ten tobacco samples and ten soil samples were tested by this method, and only one soil sample was found to contain R-indoxacarb (1.05 mg/kg) and S-indoxacarb (0.88 mg/kg). The proposed method is green, convenient and reliable for the enantioselective determination of enantiomers of indoxacarb in tobacco and soil.

关 键 词：茚虫威 手性分离 烟草 土壤 超高效合相色谱-串联质谱 

分 类 号：S482.3[农业科学—农药学] TS472[农业科学—植物保护]