Separation and determination of polyurethane amine catalysts in polyether polyols by using UHPLC–Q‐TOF‐MS on a reversed‐phase/cation‐exchange mixed‐mode column

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EarlyView Article

  • Published: Dec 21, 2017
  • Author: Jiaxiao Li, Marcel Zhu
  • Journal: Journal of Separation Science


A simple, selective, and accurate ultra‐high performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry method was established and validated for the efficient separation and quantification of polyurethane amine catalysts in polyether polyols. Amine catalysts were primarily separated in polyether polyol‐based sample by solid‐phase extraction, and further baseline separated on a reversed‐phase/cation‐exchange mixed‐mode column (SiELC Primesep™ 200) using 0.1% trifluoroacetic acid/acetonitrile as a mobile phase in gradient elution mode at a flow rate of 0.2 mL/min. High‐resolution quadrupole time‐of‐flight mass spectrometry analysis in electrospray ionization positive mode allowed the identification as N,N′‐bis[3‐(dimethylamino)propyl]urea, N‐[2‐(2‐dimethylaminoethoxy)ethyl]‐N‐methyl‐1,3‐propanediamine, and N,N,N′,N′‐tetramethyldipropylenetriamine. The method was validated and presented good linearity for all the analytes in blank matrices within the concentration range of 0.20–5.0 or 0.1–2.0 μg/mL with the correlation coefficients (R2) ranging from 0.986 to 0.997. Method recovery ranged within 81–105% at all three levels (80, 100, and 120% of the original amount) with relative standard deviations of 1.0–6.2%. The limits of detection were in the range of 0.007–0.051 μg/mL. Good precision was obtained with relative standard deviation below 3.2 and 0.72% for peak area and retention time of three amines, respectively.

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