Department IFA-Tulln, University of Natural Resources and Applied Life Sciences, Vienna, Konrad Lorenz Str. 20, A-3430 Tulln, Austria.
Anal Bioanal Chem. 2009 Nov;395(5):1355-72. doi: 10.1007/s00216-009-2995-2. Epub 2009 Aug 10.
This paper describes the application of a previously published multi-mycotoxin method for food and feed matrices based on liquid chromatography/electrospray ionization-tandem mass spectrometry (HPLC/ESI-MS/MS) to the analysis of microbial metabolites in indoor matrices. The range of investigated analytes has been extended by 99 fungal and bacterial metabolites to cover now 186 compounds overall. The method is based on a single extraction step using an acidified acetonitrile/water mixture (which has been determined to be preferable to methanol and ethyl acetate) followed by analysis of the diluted crude extract. The analytical signal of one third of the investigated analytes was reduced by more than 50% due to matrix effects in a spiked extract of house dust, whereas the other investigated materials were less critical in that aspect. For determination of method performance characteristics, a spiked reference material for house dust was chosen as a model sample for an extremely complex matrix. With few exceptions, coefficients of variation of the whole procedure of <10% and limits of detection of <50 microg kg(-1) were obtained. The apparent recoveries were below 50% for half of the investigated analytes due to incomplete extraction and/or detection-related matrix effects. The application of the method to 14 samples from damp buildings revealed the presence of 20 different analytes at concentrations of up to 130 mg kg(-1). Most of these compounds have never been identified before in real-world samples, although they are known to be produced by indoor-relevant fungi. This underlines the great value of the described method for the on-site determination of microbial metabolites.
本文描述了一种先前发表的多真菌毒素方法在食品和饲料基质中的应用，该方法基于液相色谱/电喷雾电离串联质谱（HPLC/ESI-MS/MS），用于分析室内基质中的微生物代谢产物。所研究的分析物范围已扩展到 99 种真菌和细菌代谢物，总共涵盖了 186 种化合物。该方法基于使用酸化乙腈/水混合物的单一提取步骤（已确定其优于甲醇和乙酸乙酯），然后对稀释的粗提取物进行分析。在所研究的分析物中，有三分之一的分析物由于室内灰尘提取物中的基质效应，其分析信号降低了 50%以上，而其他研究材料在这方面的影响较小。为了确定方法性能特征，选择室内灰尘标准物质作为极其复杂基质的模型样品。除了少数例外，整个程序的变异系数<10%，检测限<50μgkg(-1)。由于提取不完全和/或与检测相关的基质效应，在所研究的分析物中有一半的表观回收率低于 50%。该方法应用于 14 个潮湿建筑物的样本中，在高达 130mgkg(-1)的浓度下发现了 20 种不同的分析物。尽管这些化合物已知是由室内相关真菌产生的，但其中大多数以前从未在实际样品中被鉴定过。这突出了所描述的方法在现场测定微生物代谢产物方面的巨大价值。
