烟草中甲霜灵的手性分离方法差异研究

Investigation of Chiral Separation Methods for Metalaxyl in Tobacco

对比反相液相色谱-串联质谱(RPLC-MS/MS)和超临界流体色谱-串联质谱(SFC-MS/MS)手性分离烟草中甲霜灵的差异。烟草样品经乙腈提取、盐析分层、快速滤过型净化(multi-Plug Filtration Cleanup,m-PFC)柱净化后,分别采用RPLC-MS/MS和SFC-MS/MS进行手性分离。从多个性能参数(分离效率、线性、选择性、回收率、重复性、灵敏度、基质效应等)对两种方法进行了全面比较。采用不同的分离方法,在10~500 ng/mL范围内,甲霜灵的不同异构体均可呈现良好的线性关系(R^(2)≥0.9993)。在各异构体加标浓度为0.1、0.5、2.0 mg/kg水平下,采用不同的分离方法均可获得满意的回收率(88.7%~96.2%)和良好的重复性(RSD<7.0%)。结果表明:RPLC-MS/MS和SFC-MS/MS具有互补性,均适用于手性分离和测定烟草基质中的甲霜灵。

To investigate the differences in chiral separation of metalaxyl in tobacco,we utilized reverse phase liquid chromatography tandem mass spectrometry(RPLC-MS/MS)and supercritical fluid chromatography tandem mass spectrometry(SFC-MS/MS).Tobacco was extracted with acetonitrile,followed by salt-out with anhydrous magnesium sulfate,and purification using m-PFC(multi plug filtration cleaning)columns.Chiral separation was performed separately using RPLC-MS/MS and SFC-MS/MS.A comprehensive comparison of two methodologies was conducted based on multiple performance parameters such as separation efficiency,linearity,selectivity,recovery rate,repeatability,sensitivity,and matrix effect.The results revealed that different enantiomers of metalaxyl exhibited excellent linear relationships within the range of 10~500 ng/mL(R^(2)≥0.9993)using both separation methods.Addtionally,satisfactory recoveries(88.7%~96.2%)and good repeatability(RSD<7.0%)were achieved at levels of 0.1,0.5,and 2.0 mg/kg for each isomer when employing the different separation methods.These findings indicated that RPLC-MS/MS and SFC-MS/MS are complementary and suitable for chiral separation and determination of metalaxyl in tobacco substrates.