Separation and Quantification of Vegetable Oil Based Polyols by High Performance Liquid Chromatography with Evaporative Light Scattering Detection Jin Yue Æ Suresh S. Narine Received: 2 May 2007 / Revised: 10 July 2007 / Accepted: 12 July 2007 / Published online: 15 August 2007 Abstract Polyols with terminal primary alcohol func- tionalities were obtained from canola oil via an ozonolysis and hydrogenation process. A high performance liquid chromatography (HPLC) method with evaporative light scattering detection (ELSD) was developed for separating and quantifying the polyol products. Linear calibration curves were obtained for the mono-ol, diol and triol com- ponents with correlations (r 2 ) above 0.98. According to the standard curve, the content of mono-ol, diol and triol can be obtained from their HPLC-ELSD chromatograms. Keywords Polyol Á Canola oil Á High performance liquid chromatography Á Evaporative light scattering detection Á Calibration curve Introduction Vegetable oil is an abundant renewable source that can be used for the manufacture of polyurethanes (PUs) so long as it comprises double bonds in its structure, which can be converted to alcohol functionalities to make polyols, the monomers for polyurethane production. There are many ways to synthesize polyols from various vegetable oils. Some research groups have sought to introduce alcohol functionality by hydroformylation of double bonds [1] followed by hydrogenation or epoxidation then ring opening [1, 2]. The above mentioned methodologies have produced TAG polyols with hydroxyl functionality situated in the middle of the fatty acid chains. For the synthesis of polyols with terminal hydroxyl groups from vegetable oils, the process of ozonolysis is generally adopted [3, 4]. In our research group, a process of ozonolysis followed by hydrogenation (also demonstrated to be feasible at an industrial scale) has been successfully utilized with canola oil to make polyols with terminal hydroxyl groups [5]. These polyols are capable of producing high-quality PU foams and elastomers [6, 7]. Gel permeation chromatography (GPC) and FTIR methods were used in Petrovic’s work to characterize terminal hydroxyl polyols [3]; FTIR and 13 C-NMR were adopted in Tran’s research for characterization of similar structures [4]. Neither of these analytical methods allowed for quantification of the components of the polyols. Cur- rently, there is no literature published on the separation and quantification of different components in polyol products from vegetable oils. In this paper, we report a methodology for the separation and quantification of different compo- nents in polyols, including saturated triacylglycerols (TAGs), mono-ols, diols and a triol, utilizing high perfor- mance liquid chromatography (HPLC) and an evaporative light scattering detector (ELSD). Evaporative light scattering detection for HPLC has been widely used for the separation and quantification of lipid classes [8–16] using stationary phases of silica [17], diol [18], cyanopropyl [19], or bonded polyvinyl alcohol [20]. The use of ELSD has some advantages in the area of lipid analysis: (1) it is not sensitive to the solvent flow rate and ambient temperature [21]; (2) it eliminates the need for lipid derivatization; and (3) it allows for the use of solvents that are usually not suitable for UV detection such as chloroform, which has a similar absorbance region to the lipids [22]. J. Yue Á S. S. Narine (&) Alberta Lipid Utilization Program, Department of Agricultural Food and Nutritional Science, University of Alberta, 4-10 Agriculture/Forestry Centre, Edmonton, AB, Canada T6G 2P5 e-mail: Suresh.narine@ualberta.ca J. Yue e-mail: jiny@ualberta.ca