Development and validation of analytical method for mono, di and triacetin analysis by HPLC/UV–Vis/DAD detection with 13C NMR identification

This study aimed to synthesize sulfonated polymer resins based on styrene and trimethylolpropane triacrylate (TMPTA) and evaluate their catalytic efficiency in glycerol acetylation. A factorial design was used, with two factors, three levels, and three replicates of the center point. The factors were cross-linker percentage (YTMPTA) and cross-linker feed time (TTMPTA). Ion-exchange capacity, swelling index, and catalytic efficiency were analyzed to characterize each resin. Lower cross-linker percentages resulted in higher catalytic efficiencies, as expected. Resins synthesized with 2, 6, and 10% TMPTA had mean catalytic efficiencies of 215, 176, and 121, respectively. A linear correlation was observed between catalytic efficiency and cross-linker percentage, with R2 = 0.9971. Statistical and kinetic models were developed to represent the experimental results and support the development of strategies to improve resin formulation and synthesis conditions. TMPTA feed time at low and high levels positively influenced catalytic efficiency; the result is attributed to the micro- and macrostructure of resins. This finding was corroborated by the kinetic constants provided by the model.

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Investigation of lipolytic activity of the red king crab hepatopancreas homogenate by NMR spectroscopy

Timchenko

Molchanov

Молчанов

et al. 2022

PeerJ

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The digestive gland of craboids (hepatopancreas) is rich in a huge number of various enzymes (collagenases, nucleases, hyaluronidases, proteases), which are well studied at the moment. However, little is known about crustacean lipases. In this work, using 1H NMR spectroscopy, it was found that the hepatopancreas homogenate of the red king crab Paralithodes camtschaticus demonstrates high lipolytic activity against triacetin in a wide pH range and shows moderate activity against the caprylic/capric triglyceride emulsion. Under the action of the hepatopancreas homogenate, triacylglycerols are converted into 1,2-diacylglycerol, and then into 2-monoacylglycerol and 1-monoacylglycerol. The 1-monoacylglycerol predominates in the reaction products. The use of NMR spectroscopy makes it possible to quickly detect hydrolysis products and evaluate the reaction direction.

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Development and validation of analytical method for mono, di and triacetin analysis by HPLC/UV–Vis/DAD detection with 13C NMR identification

Cited by 3 publications

References 12 publications

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Transcending Resolution Limits in HPLC and Diffusion NMR

Synthesis of Vinyl–Trivinyl Acidic Resins for Application in Catalysis: Statistical Study and Site Accessibility Assessment

Investigation of lipolytic activity of the red king crab hepatopancreas homogenate by NMR spectroscopy

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