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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 (R ) 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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A commercial vegetable oil‐based polyol for rigid polyurethane foams has been characterized by liquid chromatography‐electrospray ionization‐quadrupole ion trap mass spectrometry (LC‐ESI‐QIT‐MS). The absolute molecular weight (MW = 960) was measured by gel permeation chromatography (GPC) equipped with both refractive index (RI) detector and static laser light‐scattering detector (SLSD), which allowed further analysis by LC‐MS. The oligo‐polyol mixture was first separated in two elutes and then investigated by a deep multistage mass spectrometry (MSn) study and completed using NMR. The major constituents identified were regioisomers of propoxylated sucrose (nPO = 6–12), and the related esters of C16:0, C18:1, and C18:2 fatty acids had a mass ratio of 6:3:1. A comparison of fatty acids composition between the sample and palm oil demonstrated that the sample was initially prepared from the mixture of sucrose and palm oil by direct propoxylation. The MSn fragmentation studies validated the structure of propoxylated sucrose and the related fatty acids derivatives. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017, 55, 255–262