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Direct electrospray ionization mass spectrometry quantitative analysis of sebacic and terephthalic acids in biodegradable polymers.

Analytical chemistry (2011-01-06)
Paola Rizzarelli, Daniela Zampino, Loredana Ferreri, Giuseppe Impallomeni
ABSTRACT

A direct, rapid, and easy electrospray ionization mass spectrometry (ESI-MS) method to determine concentrations of sebacic acid (SA) and terephthalic acid (TA) residues in biodegradable copolymers was developed. Copolyester samples were synthesized from 1,4-butanediol and sebacic and terephthalic acids by melt polymerization. Extraction of monomers was performed in methanol. Their concentrations were determined by direct infusion ESI-MS, without chromatographic separation, using 1,12-dodecanedioic acid (DDA) as an internal standard. Calibration curves were obtained by plotting the ratio of the areas of the peaks relative to monomers and DDA standard as a function of their concentration ratio. We validated the method by determining the concentration of TA residue using both the ESI-MS protocol and high-performance liquid chromatography (HPLC) analysis with UV detection. The linearity range and the detection limit of this assay were 0.1-5.0 and 0.01 ppm for SA and 0.1-6.0 and 0.03 ppm for TA. This assay represents a useful alternative to conventional methods currently employed for acid quantification, resulting advantageous for its speed and high sensitivity.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Sebacic acid, 99%
Sigma-Aldrich
Sebacic acid, ≥95.0% (GC)