Determination of Dodecanol and Short‐Chained Ethoxylated Dodecanols by LC–MS/MS (with Electrospray Ionization) After Their Derivatization (with Phenyl Isocyanate)

Abstract

This report describes the application of LC–MS/MS for the separation of dodecanol (C12OH) and homogenous fatty alcohols ethoxylated (AE) containing a dodecyl moiety and 1–9 ethoxy groups. These ethoxylates and free alcohol were derivatized for LC–MS/MS analysis with phenyl isocyanate (PIC). The derivatives of analytes with PIC were separated using a C18 column. Gradient elution with a mixture of ethyl acetate and acetonitrile (5 mM) was employed. The described determination method is characterized by low detection limits (range from 0.005 µg L−1 for: C12OH, C12EO2–7 to 1 µg L−1 for C12EO1) and quantification limits (range from 0.01 µg L−1 for: C12EO5–7 to 2 µg L−1 for C12EO1). The developed and validated method was used in combination with liquid–liquid extraction (using ethyl acetate) in order to identify and quantitatively determine the C12OH and C12EO1–9 present in environmental samples collected from Warta river water in Poznan.Graphical abstract Electronic supplementary materialThe online version of this article (doi:10.1007/s11743-017-2015-z) contains supplementary material, which is available to authorized users.

Determination of dodecanol and ethoxylated fatty alcohols from environmental samples using diatomaceous earth as a green sorbent for solid-phase extraction

“…The determination and quantification limits were optimized, improved and publish by Zembrzuska (Table ).…”

“…Derivatization of C 12 OH and C 12 EO 1‐9 with the use of PIC was described previously by Zembrzuska PIC (25.5 μL) was added to a sample containing 10 μg of C 12 OH and C 12 EO 1‐9 in 200 μL of acetonitrile. The solution was heated for 30 min at 70°C.…”

“…The methodology used for determination of C 12 OH and C 12 EO 1‐9 with PIC was previously described by Zembrzuska . LC analysis was performed using the UltiMate 3000 RSLC chromatographic system from Dionex (Sunnyvale, CA, USA).…”

“…Derivatization of C 12 OH and C 12 EO 1-9 with the use of PIC was described previously by Zembrzuska [42] PIC (25.5 μL) was added to a sample containing 10 μg of C 12 OH and C 12 EO 1-9 in 200 μL of acetonitrile. The solution was heated for 30 min at 70 • C. Then, 10 μL of methanol was added and the sample was heated again for 30 min at 70 • C. Finally, T A B L E 1 Validation data for determination of C 12 OH and C 12 EO 1-9 [42] the solution was evaporated by increasing the temperature to 80 • C. The dry residue was reconstituted in the mobile phase to a final volume of 1 mL for further LS-MS/MS analysis and filtered.…”

A novel RP‐HPLC refractive index detector method development and validation for determination of trace‐level alcohols (un‐sulfated) in sodium lauryl sulfate raw material

“…The literature describes only one method of determination using the conventional gravimetric method in the United States Pharmacopeia (Tong Liu, 2018) and a few other techniques for individual determination of components of interest by LC/LC–MS (Katayama, Masuda, & Taniguchi, 1991; Czichocki, Much, & Vollhardt, 1983; Aserin, Frenkel, & Garti, 1984; Henke & Schubert, 1980; Terol et al, 2010; Guarrasi, Mangione, Sanfratello, Martorana, & Bulone, 2010; Webster et al, 2006; Jinmao et al, 1999; Zembrzuska, 2017) and GC (Feng, Wu, & Cao, 1999). These methods did not distinguish or determine the trace mixtures of residual fatty alcohols (C 10 –C 17 ).…”