title: Flow-injection flame atomic absorption spectrometric determination of trace amounts of cadmium in solid and semisolid milk products coupling a continuous ultrasound-assisted extraction system with the online preconcentration on a chelating aminomethylphosphoric acid resin.
abstract: A new sensitive and low-cost method that combines continuous acid extraction, online preconcentration, and flame atomic absorption spectrometry for cadmium determination at microg levels in solid and semisolid milk products is described. A continuous ultrasound-assisted extraction system is used to carry out the dynamic acid extraction step. The acid extract is preconcentrated online on a minicolumn packed with a chelating resin (Chelite P, with aminomethylphosphoric acid groups), and the retained cadmium is eluted with hydrochloric acid and continuously monitored by flame atomic absorption spectrometry. An experimental design (Plackett-Burman 2-6*3/16) is used to optimize the continuous extraction and the preconcentration step. The method allowed a total sampling frequency of 28 samples/h. A good precision of the whole procedure (3.0% relative standard deviation) for a cheese sample containing 0.103 +/- 0.004 microg/g Cd (dry mass), a high enrichment factor (20.5), and detection and quantification limits of 0.014 and 0.067 microg/g, respectively, for a 60 mg of sample were obtained with this methodology. The method was successfully applied to the determination of trace amounts of cadmium in solid and semisolid milk products, such as cheese and yogurt samples.
authors.affiliation: University of Santiago de Compostela, Faculty of Chemistry, Department of Analytical Chemistry, Nutrition, and Bromatology, 15782-Santiago de Compostela, Spain.
authors.forename: Sheila
authors.initials: S
authors.lastname: Cancela
authors.forename: M Carmen
authors.initials: MC
authors.lastname: Yebra
mesh_terms: D000818:Animals; D002104:Cadmium / Q000032:analysis* / Q000737:chemistry; D002614:Chelating Agents / Q000494:pharmacology; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods*; D004305:Dose-Response Relationship, Drug; D005504:Food Analysis / Q000379:methods; D005506:Food Contamination; D006863:Hydrogen-Ion Concentration; D008892:Milk / Q000378:metabolism*; D010756:Phosphoric Acids / Q000737:chemistry; D013054:Spectrophotometry, Atomic / Q000379:methods*; D014465:Ultrasonics
chemical_list: D002614:Chelating Agents; D010756:Phosphoric Acids; D002104:Cadmium; C030242:phosphoric acid