title: Direct electrospray ionization mass spectrometry quantitative analysis of sebacic and terephthalic acids in biodegradable polymers.
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.
authors.forename: Paola
authors.initials: P
authors.lastname: Rizzarelli
authors.forename: Daniela
authors.initials: D
authors.lastname: Zampino
authors.forename: Loredana
authors.initials: L
authors.lastname: Ferreri
authors.forename: Giuseppe
authors.initials: G
authors.lastname: Impallomeni
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods; D003652:Decanoic Acids / Q000032:analysis*; D003998:Dicarboxylic Acids / Q000032:analysis*; D015394:Molecular Structure; D010795:Phthalic Acids / Q000032:analysis*; D011108:Polymers / Q000737:chemistry* / Q000378:metabolism; D021241:Spectrometry, Mass, Electrospray Ionization / Q000295:instrumentation / Q000379:methods*
chemical_list: D003652:Decanoic Acids; D003998:Dicarboxylic Acids; D010795:Phthalic Acids; D011108:Polymers; C011363:terephthalic acid; C011107:sebacic acid