Shen Shihao, Chen Min, Wang Tiannan, Fei Ting, Yang Dianhai, Cao Miaoling, Wu Da
College of Environmental Science and Engineering, Tongji University, 1239 Siping Road, Shanghai 200092, China.
Technology R&D Center, Shanghai Tobacco Group Co., Ltd., 717 Changyang Road, Shanghai 200082, China.
Int J Anal Chem. 2020 Oct 13;2020:8813142. doi: 10.1155/2020/8813142. eCollection 2020.
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 ( ) 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.
建立了一种新型的心切二维液相色谱-串联质谱联用（2D-LC-MS/MS）方法，用于烟草中灭多威残留的定性和定量分析。与传统方法相比，该方法具有相当高的灵敏度和稳定性，并且在二维液相色谱（2D-LC）方法中简化了样品处理程序。尽管灭多威在大多数反相液相色谱（RPLC）柱中的保留性能较差，但成功实施了有效的反相/反相策略。在第一维中使用XB-苯基柱有效去除基质中的数千种干扰化合物。在第二维中，使用ADME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柱直接转移到第二柱。实现了2.5 ng/mL至500 ng/mL的动态范围，相关系数（ ）大于0.9995。检测限和定量限分别确定为0.69和2.30 ng/mL。2D-LC方法对烟草样品中的灭多威具有高灵敏度、良好的重现性和回收率。因此，该新方法非常适合常规分析。
