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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

  • 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(UPC2-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5 min。②在对映体含量为2.5、7.5和15.0 mg/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50~1 000 ng/mL范围内,烟草和土壤基质中两种对映体的线性良好(R2≥0.993 2)。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0.088~0.148 mg/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(1.05 mg/kg)和S-茚虫威(0.88 mg/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。

     

    Abstract: 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 (UPC2-MS/MS). Sample preparation prior to UPC2-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 (R2 ≥ 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.

     

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