Rapid, simplified microscale quantitative analysis of lignin H/G/S composition with GC–MS in glass ampules and glass capillaries

Q Qi,Jiaqi Hu,Long Qu,Xiangning Jiang,Yang Gai,Sofia A Valenzuela,Liwang Qi

doi:10.1016/j.mex.2019.11.005

Q Qi, Jiaqi Hu + Show 5 more

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https://doi.org/10.1016/j.mex.2019.11.005

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The characterization of monolignols H-, G- and S- units composition Vanholme et al. (2010) of lignin is important in agriculture, forestry, herb medicine, livestock, and health care research Vanholme et al. (2008) and Sticklen (2008). The conventional methods often require a great deal of samples and reagents and are time-consuming. Here, we present a newly developed method with fewer operations. The optimized method is suitable for detecting and characterizing lignin composition of cell wall in different plant species and has the advantages of:•Avoiding the influence of plasticizer by plasticware and enhancing the accuracy of monolignols analysis.•Lowering the required samples from grams to milligrams, and organic reagents from milliliters to microliters.•Reducing the time required from a few days to 6 h.

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Thioacidolysis is a powerful method, there are some drawbacks, which include (1) high minimum sample amounts required, (2) some harmful effects of ethanethiol, a major ingredient, on operators, (3) contaminating effects of organic reagents on the environment, (4) possible plasticizers and dyes on interfering substances by plastics, and (5) possible leaks from caps and decreases of product yields
A new method that is simple, rapid, precise, environmentally friendly and applicable at microscale is required. These are reflected in the optimized method of our study that refined the conventional thioacidolysis method to reduce sample requirement and reagent consumption, simplify operations, and produce high reaction yields and more reproducible results
Because BSTFA is especially sensitive to moisture, the silylation with BSTFA needs to be conducted in an anhydrous environment. This requires the organic extraction of thioacidolysis products being dried with desiccants (e.g., Na2SO4), which minimizes water influence, but results in sample loss

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Introduction

Thioacidolysis is a powerful method, there are some drawbacks, which include (1) high minimum sample amounts required, (2) some harmful effects of ethanethiol, a major ingredient, on operators, (3) contaminating effects of organic reagents on the environment, (4) possible plasticizers and dyes on interfering substances by plastics, and (5) possible leaks from caps and decreases of product yields. These are reflected in the optimized method of our study that refined the conventional thioacidolysis method to reduce sample requirement and reagent consumption, simplify operations, and produce high reaction yields and more reproducible results.

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