Department of Chemistry, University of Waterloo, Waterloo, Ontario, Canada.
J Chromatogr A. 2013 Oct 25;1313:139-46. doi: 10.1016/j.chroma.2013.07.071. Epub 2013 Jul 23.
A fast and robust method was developed for the determination of ten triazole fungicides in fruit samples using direct immersion solid-phase microextraction coupled to gas chromatography with time-of-flight mass spectrometry detection (DI-SPME-GC-ToFMS). In this work, a newly developed concept of solid-phase microextraction (SPME) sorbent, which allows for direct immersion extraction in complex food matrices, has been applied in the analysis of 10 triazole fungicides in grapes and strawberries pulps. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction temperature, sample pH, and ionic strength, agitation speed, extraction and desorption times. Under optimized conditions, the method was linear for over 4 orders of magnitude in concentration, with linear regression coefficients (R(2)) greater than 0.99 for all test compounds in both matrices. Method reproducibility, as determined by analysis of spiked grapes and strawberries, was better than ±20%. The limits of quantitation objective (LOQs) ranged from 0.25 to 5 ng g(-1) for both matrices, well below the maximum residues levels allowed for those compounds in both matrices. The method was successfully applied in the analysis of commercial samples of grapes and strawberries. Finally, the new SPME method was compared to a modified version of t QuEChERS AOAC method: the limits of quantitation reached by SPME were at least one order of magnitude lower than those achieved by the QuEChERS method, whereas precision and accuracy were comparable for both methods.
建立了一种快速、稳健的方法,用于使用直接浸入固相微萃取(DI-SPME)与气相色谱-飞行时间质谱联用(GC-ToFMS)检测,对水果样品中的十种三唑类杀菌剂进行测定。在这项工作中,应用了一种新开发的固相微萃取(SPME)吸附剂的概念,该吸附剂允许在复杂的食品基质中直接浸入萃取,用于分析葡萄和草莓浆中的十种三唑类杀菌剂。考察并优化了影响萃取效率的潜在因素,包括萃取温度、样品 pH 值和离子强度、搅拌速度、萃取和解析时间。在优化条件下,该方法在两种基质中浓度超过 4 个数量级的范围内呈线性,所有测试化合物的线性回归系数(R²)均大于 0.99。通过对葡萄和草莓的加标分析,确定方法的重现性优于±20%。两种基质的定量限(LOQs)均为 0.25-5ng g⁻¹,远低于两种基质中允许的这些化合物的最大残留限量。该方法成功应用于商业葡萄和草莓样品的分析。最后,将新的 SPME 方法与改良版的 QuEChERS AOAC 方法进行了比较:SPME 的定量限至少比 QuEChERS 方法低一个数量级,而两种方法的精密度和准确度相当。