College of Science, China Agricultural University, Beijing, P. R. China.
J Sep Sci. 2012 Jan;35(1):166-73. doi: 10.1002/jssc.201100365. Epub 2011 Nov 21.
A sensitive and rapid analytical method was developed for simultaneous determination of triadimefon (TF) and triadimenol (TN) stereoisomers in wheat, straw, and soil by liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS/MS). The direct enantioseparation of TF and TN was performed on a Lux cellulose-1 column packed with cellulose-tris-(3,5-dimethylphenylcarbamate). The effects of mobile-phase composition on the separation were investigated and stereoisomeric elution orders were confirmed with a polarimeter detector. The pesticides were extracted from samples with acetonitrile and cleaned up by solid-phase extraction or activated carbon. Based on the developed stereoselective LC-MS/MS method, for TF and TN stereoisomers, good linearities were obtained over the concentration range of 0.003-4 mg/L; recoveries were 84.2-102.7% in wheat, 84.0-104.0% in straw, and 85.2-106.8% in soil at spiked concentrations of 0.007-2.0 mg/kg; intra-day and inter-day assay precisions were below 12.2%. Limits of detection (LODs) and limits of quantification (LOQs) in wheat, straw, and soil were 0.001-0.005 mg/kg and 0.007-0.02 mg/kg, respectively. Finally, the method was successfully applied to detect TF and TN stereoisomers in wheat, straw, and soil samples from residual trials in farm.
建立了一种同时测定小麦、秸秆和土壤中三唑酮（TF）和三唑醇（TN）对映异构体的灵敏、快速分析方法。采用手性 Lux 纤维素-1 柱（填充纤维素-三-（3,5-二甲基苯基氨基甲酸酯））对 TF 和 TN 进行直接对映体分离。考察了流动相组成对分离的影响，并通过旋光检测器确定了对映异构体的洗脱顺序。采用乙腈提取样品中的农药，并用固相萃取或活性炭进行净化。基于开发的立体选择性 LC-MS/MS 方法，TF 和 TN 对映异构体在 0.003-4 mg/L 的浓度范围内具有良好的线性；在 0.007-2.0 mg/kg 浓度下，小麦、秸秆和土壤中的回收率为 84.2-102.7%、84.0-104.0%和 85.2-106.8%；日内和日间测定精密度均低于 12.2%。小麦、秸秆和土壤中的检测限（LOD）和定量限（LOQ）分别为 0.001-0.005 mg/kg 和 0.007-0.02 mg/kg。最后，该方法成功应用于残留试验中农田小麦、秸秆和土壤样品中 TF 和 TN 对映异构体的检测。
