采用固相萃取和高效液相色谱-大气压化学电离质谱法测定葡萄酒中的唑类杀菌剂。

Determination of azolic fungicides in wine by solid-phase extraction and high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

作者信息

Nozal Maria J, Bernal J L, Jiménez J J, Martín Maria T, Bernal J

机构信息

Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid, Prado de la Magdalena s/n, E-47005 Valladolid, Spain.

出版信息

J Chromatogr A. 2005 May 27;1076(1-2):90-6. doi: 10.1016/j.chroma.2005.04.044.

DOI:10.1016/j.chroma.2005.04.044

PMID:15974073

Abstract

A method for simultaneous analysis of eight azolic fungicides: cyproconazole, diniconazole, tetraconazole, thiabendazole, flusilazole, triadimenol, triadimefon, carbendazim and the degradation product 2-aminobenzimidazole in wine samples is described. The compounds are isolated from the samples and concentrated by solid-phase extraction on polymeric cartridges. The determination is carried out by liquid chromatography with mass spectrometric detection in positive ionization and selected ion monitoring modes. The influence of parameters such as the mobile phase composition, column temperature, corona current and fragmentor voltage is studied and the proposed method is validated. Recoveries of the nine compounds added to wine samples range from 83 to 109%, with relative standard deviations below 10%. The quantitation limits are between 9 and 31 microg/L. Real wine samples are analyzed by the proposed method, also.

摘要

描述了一种同时分析葡萄酒样品中8种唑类杀菌剂的方法，这8种杀菌剂分别为：环丙唑醇、烯唑醇、四氟醚唑、噻菌灵、氟硅唑、三唑醇、三唑酮、多菌灵及其降解产物2-氨基苯并咪唑。这些化合物从样品中分离出来，并通过在聚合物柱上进行固相萃取进行浓缩。采用液相色谱-质谱检测，在正离子化和选择离子监测模式下进行测定。研究了流动相组成、柱温、电晕电流和碎裂电压等参数的影响，并对所提出的方法进行了验证。添加到葡萄酒样品中的9种化合物的回收率在83%至109%之间，相对标准偏差低于10%。定量限在9至31μg/L之间。所提出的方法也用于分析实际葡萄酒样品。