A novel heart-cutting two-dimensional liquid chromatography coupled with tandem mass spectrometry (2D-LC-MS/MS) was developed for the qualitative and quantitative analysis of methomyl residue in tobacco. Compared to traditional methodologies, fairly high sensitivity and stability were achieved, and the sample procedure was simplified in the two-dimensional liquid chromatography (2D-LC) method. Although methomyl had poor retention performance in most of the reversed-phase liquid chromatography (RPLC) columns, an effective RP/RP strategy was successfully facilitated. An XB-Phenyl column was employed in the first dimension to effectively remove thousands of interference compounds in the matrix. In the second dimension, an ADME column was applied for further separation. After optimization of the separation conditions, a six-way valve was utilized for direct transformation of the target fraction from the 1st column to the 2nd column. A dynamic range of 2.5 ng/mL to 500 ng/mL was achieved with correlation coefficient (r²) greater than 0.9995. The limit of detection and limit of quantification were determined to be 0.69 and 2.30 ng/mL, respectively. The 2D-LC method shows high sensitivity, good reproducibility, and recovery for methomyl in tobacco samples. Therefore, the new method was quite suitable for routine analysis.

中文翻译：

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串联质谱联用心切割二维液相色谱法测定烟草样品中的甲基甲酚残留

开发了一种新颖的中心切割二维液相色谱-串联质谱（2D-LC-MS / MS），用于烟草中甲胺基残留的定性和定量分析。与传统方法相比，二维液相色谱（2D-LC）方法获得了相当高的灵敏度和稳定性，并且简化了采样程序。尽管灭多威在大多数反相液相色谱（RPLC）色谱柱中保留性能较差，但成功地促进了有效的RP / RP策略。在第一维中使用了XB-苯基柱，以有效去除基质中的数千种干扰化合物。在第二维中，使用ADME色谱柱进行进一步分离。优化分离条件后，使用六通阀将目标馏分从第一塔直接转化为第二塔。动态范围为2.5 ng / mL至500 ng / mL，相关系数为（r ²）大于0.9995。检测限和定量限分别确定为0.69和2.30 ng / mL。二维液相色谱法显示了高灵敏度，良好的重现性和烟草样品中甲虫基的回收率。因此，该新方法非常适合常规分析。