Rial Otero R, Yagüe Ruiz C, Cancho Grande B, Simal Gándara J
Analytical and Food Chemistry Department, Faculty of Food Science and Technology, University of Vigo, Ourense, Spain.
J Chromatogr A. 2002 Jan 4;942(1-2):41-52. doi: 10.1016/s0021-9673(01)01352-8.
A solid-phase microextraction (SPME) followed by a gas chromatographic-mass spectrometric (GC-MS) determination has been developed and validated for the determination of cyprodinil and fludioxonil in white wine samples. Extraction parameters such as the selection of SPME coating, the effect of the temperature, the effect of the headspace volume and the salt addition were studied and optimized, together with GC-MS analytical conditions. The divinylbenzene-Carboxen-polydimethylsiloxane (DVB-CAR-PDMS) fiber was the most appropriate for the determination of the two pesticides in wine. The quality parameters of the proposed method demonstrated a good precision (RSD about 5%), with detection limits of 0.1 and 0.2 microg/l for cyprodinil and fludioxonil, respectively. Fifteen commercial white wine samples produced in Rías Baixas area in Galicia (N.W. Spain) were analyzed with the SPME-GC-MS procedure. Some of the commercial wines (75%) presented the two pesticides in concentrations ranging from 0.9 to 28.6 microg/l. In conclusion, SPME-GC-MS has a great potential for fungicide determination in wines.
已开发并验证了一种采用固相微萃取（SPME）结合气相色谱 - 质谱联用（GC - MS）测定白葡萄酒样品中嘧菌环胺和咯菌腈的方法。研究并优化了萃取参数，如SPME涂层的选择、温度的影响、顶空体积的影响以及盐添加的影响，同时还优化了GC - MS分析条件。二乙烯基苯 - 碳分子筛 - 聚二甲基硅氧烷（DVB - CAR - PDMS）纤维最适合用于测定葡萄酒中的这两种农药。所提出方法的质量参数显示出良好的精密度（相对标准偏差约为5%），嘧菌环胺和咯菌腈的检测限分别为0.1和0.2微克/升。采用SPME - GC - MS程序分析了加利西亚（西班牙西北部）下海湾地区生产的15个商业白葡萄酒样品。部分商业葡萄酒（75%）中这两种农药的浓度范围为0.9至28.6微克/升。总之，SPME - GC - MS在葡萄酒中杀菌剂测定方面具有很大潜力。
