Jump to main content
Jump to site search


1H NMR determination of 1, 3-dicyclohexylurea, glutaric acid and triethylamine in medical four-arm poly (ethylene glycol)-N-hydroxysuccinimide-glutarate for better quality control

Abstract

Absorbable vascular sealing medical glue, which belongs to the Class III medical device, is a special new material for preventing the leakage of cerebrospinal fluid. Medical four-arm poly (ethylene glycol)-N-hydroxysuccinimide-glutarate (4-arm-PEG-SG) with molecular weight of 20,000 is the main component of the absorbable medical glue. According to its quality standard, the quality control of the residues 1, 3-dicyclohexylurea (DCU), glutaric acid (GA) and triethylamine (TEA) is required. A rapid analytical method by quantitative 1H nuclear magnetic resonance (1H NMR) for the determination of residues DCU, GA and TEA in medical 4-arm-PEG-SG was established in the present study. The peaks at δ1.56 (4H, m), δ2.71 (4H, t, J = 6.7 Hz), δ2.42 (6H, q, J = 7.2 Hz) were selected for quantifying the DCU, GA and TEA, respectively, with deuterated pyridine as the solvent and tetramethylsilane as the internal standard. The 1H NMR assay was validated by several experimental parameters including specificity, linearity, accuracy, precision, robustness, limit of detection (LOD), limit of quantification (LOQ) and stability. The average recoveries obtained were in the range of 99.48 – 102.02% for all the three residues. Compared with the HPLC and GC approach, the proposed 1H NMR method proved to be a powerful tool for quantification due to its unique advantages of simple, rapid and high robustness, especially on not requiring standard compounds for calibration curve preparation.

Back to tab navigation

Supplementary files

Publication details

The article was received on 10 Jul 2019, accepted on 05 Nov 2019 and first published on 06 Nov 2019


Article type: Paper
DOI: 10.1039/C9AY01471C
Anal. Methods, 2019, Accepted Manuscript

  •   Request permissions

    1H NMR determination of 1, 3-dicyclohexylurea, glutaric acid and triethylamine in medical four-arm poly (ethylene glycol)-N-hydroxysuccinimide-glutarate for better quality control

    S. Wang, F. Li, H. liu and Y. zhang, Anal. Methods, 2019, Accepted Manuscript , DOI: 10.1039/C9AY01471C

Search articles by author

Spotlight

Advertisements