Tao Yan, Zheng Zuntao, Yu Yang, Xu Jun, Liu Xingang, Wu Xiaohu, Dong Fengshou, Zheng Yongquan
State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China.
Institute for the Control of Agrochemicals, Ministry of Agriculture, Beijing 100125, PR China.
Food Chem. 2018 Feb 15;241:32-39. doi: 10.1016/j.foodchem.2017.08.038. Epub 2017 Aug 14.
Here, we developed a rapid and robust supercritical fluid chromatography-tandem mass spectrometry (SFC-MS/MS) method for simultaneous detection of fenbuconazole and its chiral metabolites in fruit, vegetable, cereal, and soil. Baseline separation of six stereoisomers was achieved on an amylose tris-(3,5-dimethylphenylcarbamate)-coated chiral column in 4.0min using a mobile phase composed of CO/ethanol (flow rate of 1.8mL/min). Ionisation efficiency and sensitivity was optimized with a post-column compensation solvent (0.1% formic acid/methanol). Target analytes were extracted with acetonitrile and purified using dispersive solid phase extraction sorbents. Six stereoisomers at three concentrations (5, 50, and 250µg/kg) achieved satisfactory recoveries (76.3-104.6%) with RSDs≤11.5% Excellent linearities (R≥0.9963) and the limits of quantification (LOQs, 0.13-3.31μg/kg) were established for all six stereoisomers. Results show that the proposed method is suitable for routine detection of six stereoisomers of fenbuconazole and its chiral metabolites in food and environmental samples.
在此,我们开发了一种快速且可靠的超临界流体色谱-串联质谱(SFC-MS/MS)方法,用于同时检测水果、蔬菜、谷物和土壤中的苯醚甲环唑及其手性代谢物。使用由CO/乙醇(流速为1.8mL/min)组成的流动相,在直链淀粉三(3,5-二甲基苯基氨基甲酸酯)涂覆的手性柱上于4.0分钟内实现了六种立体异构体的基线分离。通过柱后补偿溶剂(0.1%甲酸/甲醇)优化了电离效率和灵敏度。目标分析物用乙腈萃取,并使用分散固相萃取吸附剂进行纯化。三种浓度(5、50和250μg/kg)的六种立体异构体实现了令人满意的回收率(76.3 - 104.6%),相对标准偏差≤11.5%。为所有六种立体异构体建立了出色的线性关系(R≥0.9963)和定量限(LOQs,0.13 - 3.31μg/kg)。结果表明,所提出的方法适用于食品和环境样品中苯醚甲环唑六种立体异构体及其手性代谢物的常规检测。