Institute of Clinical Chemistry and Laboratory Medicine, University Hospital Regensburg, Franz-Josef-Strauß-Allee 11, 93053, Regensburg, Germany.
Department of Nutrition, Exercise and Sports, Faculty of Science, University of Copenhagen, Nørre Allé 51, 2200, Copenhagen, Denmark.
Anal Bioanal Chem. 2020 Apr;412(10):2315-2326. doi: 10.1007/s00216-020-02416-y. Epub 2020 Mar 21.
The intestinal microbiome plays an important role in human health and disease and fecal materials reflect the microbial activity. Thus, analysis of fecal metabolites provides insight in metabolic interactions between gut microbiota and host organism. In this work, we applied flow injection analysis coupled to Fourier transform mass spectrometry (FIA-FTMS) to identify and quantify lipid species in human fecal samples. Fecal homogenates were subjected to lipid extraction and analyzed by FIA-FTMS. The analysis of different subjects revealed a vast heterogeneity of lipid species abundance. The majority of samples displayed prominent signals of triacylglycerol (TG) and diacylglycerol (DG) species that could be verified by MS2 spectra. Therefore, we focused on the quantification of TG and DG. Method validation included limit of quantification, linearity, evaluation of matrix effects, recovery, and reproducibility. The validation experiments demonstrated the suitability of the method, with exception for approximately 10% of samples, where we observed coefficients of variation higher than 15%. Impaired reproducibility was related to sample inhomogeneity and could not be improved by additional sample preparation steps. Additionally, these experiments demonstrated that compared with aqueous samples, samples containing isopropanol showed higher amounts of DG, presumably due to lysis of bacteria and increased TG lipolysis. These effects were sample-specific and substantiate the high heterogeneity of fecal materials as well as the need for further evaluation of pre-analytic conditions. In summary, FIA-FTMS offers a fast and accurate tool to quantify DG and TG species and is suitable to provide insight into the fecal lipidome and its role in health and disease.
肠道微生物群在人类健康和疾病中起着重要作用,粪便材料反映了微生物的活性。因此,分析粪便代谢物可以深入了解肠道微生物群与宿主之间的代谢相互作用。在这项工作中,我们应用流动注射分析与傅里叶变换质谱联用(FIA-FTMS)来鉴定和定量人粪便样本中的脂质种类。将粪便匀浆进行脂质提取并通过 FIA-FTMS 进行分析。对不同个体的分析显示,脂质种类的丰度存在很大的异质性。大多数样本显示出显著的三酰基甘油(TG)和二酰基甘油(DG)信号,可以通过 MS2 谱进行验证。因此,我们专注于 TG 和 DG 的定量分析。方法验证包括定量下限、线性、基质效应评价、回收率和重现性。验证实验表明该方法适用性良好,但大约 10%的样本存在问题,其变异系数高于 15%。重现性差与样品不均匀有关,通过额外的样品制备步骤无法改善。此外,这些实验表明,与水相样品相比,含有异丙醇的样品显示出更高的 DG 含量,可能是由于细菌裂解和 TG 脂肪水解增加所致。这些影响是样品特异性的,证实了粪便材料的高度异质性以及进一步评估分析前条件的必要性。总之,FIA-FTMS 提供了一种快速准确的定量 DG 和 TG 种类的工具,适合深入了解粪便脂质组及其在健康和疾病中的作用。