In contrast to isolated molecules such as purified natural products or proteins in laboratory system, the substantial world such as human being or nature undoubtedly consist many molecular mixtures in solids, solution and gas-phase. We are challenging to analyze biomolecular mixtures in natural environment . For example, plant biomass consists polysaccharides and lignin, these difficulties by tackling NMR are attributed to low solubility, mixture complexity and limited spectral dispersion. Firstly we tried several solid-state NMR measurements (CP/MAS, 2D-INADEQUATE and DARR) followed with multivariate analysis, enabled successful characterization of structural variations between ionic-liquids solubilized and regenerated cellulose . Furthermore, newly developed 2D- dipolar dephasing filtered INADEQUATE and DARR exhibited selective detection of hemicellulose signals using lignocellulose solid mixture samples . Next subject should be tackling to monitor biomass degradation process in natural or industrial microbiota. Therefore we applied multi-variate and statistical correlation analysis for degraded metabolite mixture data observed in the microbiota. Namely, time-dependent analysis of cellulosic degradation in paddy soil , as well as methane fermentation sludge , demonstrated “discovery of biomarker concept” in environmental science.