Department of Chemistry, University of La Rioja, Madre de Dios, 51, 26006 Logroño, Spain.
J Chromatogr A. 2012 Dec 28;1270:62-71. doi: 10.1016/j.chroma.2012.10.069. Epub 2012 Nov 6.
Four different methods for simultaneous extraction of vinclozolin, dichlofluanid, penconazole, captan, quinoxyfen, fluquinconazol, boscalid and pyraclostrobin from grapes were optimized and further tested. Microwave assisted extraction (MAE), matrix solid-phase dispersion (MSPD), solid-liquid extraction (SLE) and QuEChERS were compared in terms of their limits of detection and quantification and recoveries. For MAE, MSPD and ethyl acetate extraction, the optimal conditions were optimized by using experimental designs. The analysis was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode (GC-MS, SIM). The proposed methods showed good sensitivity, limits of quantification were lower than MRLs and precision (expressed as relative standard deviation) ranged from 2.9 to 11.1%. The recoveries obtained from MAE, MSPD, SLE and QuEChERS were in the range 78-100%, 66-102%, 58-88% and 68-96%, respectively. In addition, the four methods were compared in two ways: by means of calibration curves obtained with 10 fortified samples in the studied range of concentrations and by the application of statistical tests such as Levene's test (to study variance homogeneity), ANOVA and Tukey's test (in case of Levene's test was satisfactory) for the assessment of the information obtained in the analysis of real samples. Both ways of comparison led to the same results: no differences between the four methods for the extraction of vinclozolin, dichofluanid, quinoxyfen, fluquinconazol and pyraclostrobin were found. However, there were differences for the analysis of captan, boscalid and penconazole.
从葡萄中同时提取 Vinclozolin、Dichlofluanid、Penconazole、Captan、Quinoxyfen、Fluquinconazole、Boscacid 和 Pyraclostrobin 的四种不同方法进行了优化和进一步测试。微波辅助提取（MAE）、基质固相分散（MSPD）、固液萃取（SLE）和 QuEChERS 在检测限和定量限以及回收率方面进行了比较。对于 MAE、MSPD 和乙酸乙酯提取，通过实验设计优化了最佳条件。使用气相色谱-质谱法在选择离子监测模式（GC-MS，SIM）下进行分析。所提出的方法具有良好的灵敏度，定量限低于 MRL，精密度（表示为相对标准偏差）在 2.9%至 11.1%之间。MAE、MSPD、SLE 和 QuEChERS 的回收率分别在 78%-100%、66%-102%、58%-88%和 68%-96%之间。此外，通过用在研究浓度范围内的 10 个加标样品获得的校准曲线以及通过应用统计测试（如 Levene 检验（用于研究方差同质性）、方差分析和 Tukey 检验（在 Levene 检验令人满意的情况下）对实际样品分析中获得的信息进行评估，对这四种方法进行了两种方式的比较。这两种比较方式都得出了相同的结果：对于 Vinclozolin、Dichlofluanid、Quinoxyfen、Fluquinconazol 和 Pyraclostrobin 的提取，这四种方法之间没有差异。然而，在 Captan、Boscacid 和 Penconazole 的分析方面存在差异。
