Navalón Alberto, Prieto Avismelsi, Araujo Lilia, Vílchez José Luis
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avda. Fuentenueva s/n, E-18071 Granada, Spain.
J Chromatogr A. 2002 Nov 1;975(2):355-60. doi: 10.1016/s0021-9673(02)01220-7.
A method for determination of trace amounts of the fungicides pyrimethanil and kresoxim-methyl in green groceries, previous headspace solid-phase microextraction (HSSPME), was developed using gas chromatography-mass spectrometry and selected ion monitoring (GC-MS, SIM). Both fungicides were extracted with a fused-silica fiber coated with 85 microm polyacrylate. The effects of pH, ionic strength, extraction and desorption times as well as the extraction temperature were studied. The linear concentration range of application was 12.5-250 ng g(-1) for both compounds, with detection limits of 1.8-2.0 ng g(-1) for pyrimethanil and 2.8-3.1 ng g(-1) for kresoxim-methyl. SPME/GC-MS analysis yielded good reproducibility (RSD between 7.4 and 15.0%). It was applied to check the eventual existence of pyrimethanil and kresoxim-methyl above the detection limits on grapes, strawberries, tomatoes and ketchup samples. The method validation was completed with spiked matrix samples. It can be applied as a monitoring tool in grapes, strawberries, tomatoes and ketchup samples.
建立了一种使用气相色谱 - 质谱联用仪和选择离子监测（GC - MS，SIM）测定蔬菜水果中痕量杀菌剂嘧霉胺和醚菌酯的方法，即顶空固相微萃取（HSSPME）法。两种杀菌剂均用涂有85μm聚丙烯酸酯的熔融石英纤维进行萃取。研究了pH值、离子强度、萃取和解吸时间以及萃取温度的影响。两种化合物的线性应用浓度范围均为12.5 - 250 ng g⁻¹，嘧霉胺的检测限为1.8 - 2.0 ng g⁻¹，醚菌酯的检测限为2.8 - 3.1 ng g⁻¹。SPME/GC - MS分析具有良好的重现性（相对标准偏差在7.4%至15.0%之间）。该方法用于检测葡萄、草莓、番茄和番茄酱样品中嘧霉胺和醚菌酯是否存在高于检测限的情况。通过加标基质样品完成了方法验证。该方法可作为葡萄、草莓、番茄和番茄酱样品的监测工具。
