Antonio Ananda da Silva, Aguiar Ana Tayná Chaves, Dos Santos Gustavo Ramalho Cardoso, Pereira Henrique Marcelo Gualberto, da Veiga-Junior Valdir Florêncio, Wiedemann Larissa Silveira Moreira
Chemistry Department, Institute of Exact Sciences, Federal University of Amazonas Avenida Rodrigo Octávio, 6200, Coroado CEP: 69.077-000 Manaus AM Brazil
Federal University of Rio de Janeiro, Chemistry Institute, Brazilian Doping Control Laboratory (LBCD - LADETEC/IQ - UFRJ) Avenida Horácio Macedo, 1281 - Pólo de Química - Cidade Universitária, Ilha do Fundão CEP: 21941-598 Rio de Janeiro RJ Brazil.
RSC Adv. 2020 Jan 21;10(6):3459-3471. doi: 10.1039/c9ra10436d. eCollection 2020 Jan 16.
Untargeted metabolomics aim to provide a global chemical fingerprint of biological matrices. This research field can be used in phytochemical screenings for bioactive species or in the identification of species. Despite its importance in providing a global chemical profile, little research has focused on the optimization of the extraction methods, as each type of matrix requires a specific procedure. Therefore, we propose to evaluate the effect of different extraction features in an ultrasound-assisted extraction for the untargeted metabolomic study of an species, a genus of great economical interest but little chemical exploitation. Method optimization was performed in a full factorial 23 design, evaluating the solvent composition, extraction temperature, sample particle size and sample : solvent ratio effects in the metabolomic response. The effect of these parameters on the quality of the untargeted metabolomic profiles was studied by analysis of the extraction yield as well as the chromatographic and spectrometric profiles. Most substances identified were glycosylated flavonoids and aporphinic alkaloids. The application of 70% ethanol enhanced the extraction of several specialized metabolites. Statistical analysis of extraction yield and chemical profiles indicates that high temperatures and low proportion between sample and extracting solvent reduce the quality and modify the chemical profile, both qualitatively and quantitatively. The use of 70% ethanol as the extracting solvent, 1 : 12 sample : solvent ratio, 40 °C as the extraction temperature and particle size of 0.595 mm were the optimized conditions to produce a comprehensive chemical profile for .
非靶向代谢组学旨在提供生物基质的整体化学指纹图谱。该研究领域可用于生物活性物质的植物化学筛选或物种鉴定。尽管其在提供整体化学概况方面很重要，但很少有研究关注提取方法的优化，因为每种类型的基质都需要特定的程序。因此，我们建议评估不同提取特征在超声辅助提取中对一种具有重大经济价值但化学开发较少的属植物进行非靶向代谢组学研究的影响。方法优化采用全因子2³设计进行，评估溶剂组成、提取温度、样品粒径和样品与溶剂比例对代谢组学响应的影响。通过分析提取产率以及色谱和光谱图谱，研究了这些参数对非靶向代谢组学图谱质量的影响。鉴定出的大多数物质为糖基化黄酮类化合物和阿朴菲生物碱。70%乙醇的应用提高了几种特殊代谢产物的提取率。提取产率和化学图谱的统计分析表明，高温和样品与提取溶剂之间的低比例会降低质量，并在定性和定量方面改变化学图谱。使用70%乙醇作为提取溶剂、1:12的样品与溶剂比例、40°C作为提取温度以及0.595mm的粒径是为该植物生成全面化学图谱的优化条件。
