School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, P.R. China.
School of Pharmaceutical Engineering, Shenyang Pharmaceutical University, Shenyang, P.R. China.
J Sep Sci. 2017 Aug;40(16):3257-3266. doi: 10.1002/jssc.201700250. Epub 2017 Jul 21.
A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained.
一种新颖可靠的方法，用于测定中药样品中五种三唑类杀菌剂残留（三唑酮、戊唑醇、烯唑醇、氟环唑和己唑醇），采用分散固相萃取结合超声辅助分散液液微萃取，然后进行超高效液相色谱-串联质谱分析。通过直接向萃取溶液中加入吸附剂，进行分散固相萃取来净化提取物，然后进行摇晃和离心。之后，迅速将 400 μL 三氯甲烷（萃取溶剂）和 0.5 mL 上述上清液的混合物注入水中，进行分散液液微萃取程序。优化了影响萃取效率的因素。在最佳条件下，校准曲线在 2.0-400ng/g（戊唑醇、烯唑醇和己唑醇）和 4.0-800ng/g（三唑酮和氟环唑）范围内具有良好的线性关系，相关系数均高于 0.9958。本方法的检出限和定量限分别为 0.5-1.1 和 1.8-4.0ng/g。目标分析物的回收率在 80.2%至 103.2%之间。该方法已成功应用于中药样品中五种三唑类杀菌剂的分析，取得了满意的结果。
