title: Headspace-single drop microextraction (HS-SDME) in combination with high-performance liquid chromatography (HPLC) to evaluate the content of alkyl- and methoxy-phenolic compounds in biomass smoke.
abstract: The content of ten phenolic compounds present in four different biomass smoke materials: rock rose (Cistus monpelienisis), prickly pear (Opuntia ficus indica), pine needles (Pinus canariensis), and almonds skin (Prunus dulcis), have been evaluated. The sampling method mainly consisted of a trap alkaline solution to solubilize the phenols, and was optimized by an experimental design. Average sampling efficiencies of 78.1% and an average precision value of 10.6% (as relative standard deviation, RSD), were obtained for the selected group of phenols. The trapped phenolates were further analyzed by a headspace-single drop microextraction (HS-SDME) procedure, in combination with high-performance liquid chromatography (HPLC) with UV detection. The optimum variables for the HS-SDME method were: 1-decanol as extractant solvent, 3.5 μL of microdrop volume, 2 mL of sample volume, a pH value of 2, saturation of NaCl, an extraction temperature of 60°C, and an extraction time of 25 min. The optimized HS-SDME method presented detection limits ranging from 0.35 to 5.8 μg mL(-1), RSD values ranging from 0.7 to 7.4%, and an average relative recovery (RR) of 99.8% and an average standard deviation of 5.2. The average content of phenolic compounds in the biomass materials studied were 70, 161, 206 and 252 mg kg(-1) of biomass for prickly pear, almonds skin, rock rose, and pine needles, respectively. The main components of the smokes were vanillin, phenol and methoxyphenols, in all smoking materials studied.
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Universidad de La Laguna (ULL), La Laguna (Tenerife), Spain.
authors.forename: Arturo A
authors.initials: AA
authors.lastname: Rincón
authors.forename: Verónica
authors.initials: V
authors.lastname: Pino
authors.forename: Juan H
authors.initials: JH
authors.lastname: Ayala
authors.forename: Ana M
authors.initials: AM
authors.lastname: Afonso
mesh_terms: D001547:Benzaldehydes / Q000032:analysis / Q000737:chemistry; D018533:Biomass; D029421:Cactaceae / Q000737:chemistry / Q000254:growth & development; D002623:Chemistry Techniques, Analytical / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005421:Flavoring Agents / Q000032:analysis / Q000737:chemistry; D010636:Phenols / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D028223:Pinus / Q000737:chemistry / Q000254:growth & development; D063245:Plant Development; D010944:Plants / Q000737:chemistry*; D027861:Prunus / Q000737:chemistry / Q000254:growth & development; D012906:Smoke / Q000032:analysis*
chemical_list: D001547:Benzaldehydes; D005421:Flavoring Agents; D010636:Phenols; D012906:Smoke; C100058:vanillin