title: Stir-membrane solid-liquid-liquid microextraction for the determination of parabens in human breast milk samples by ultra high performance liquid chromatography-tandem mass spectrometry.
abstract: In this article, stir-membrane solid-liquid-liquid microextraction (SM-SLLME) is tailored for the analysis of solid matrices and it has been evaluated for the determination of parabens in l breast milk samples. A three-phase microextraction mode was used for the extraction of the target compounds taking advantage of their acid-base properties. The unit allows the simultaneous extraction of the target compounds from the solid sample to an organic media and the subsequent transference of the analytes to an aqueous acceptor phase. The method includes the identification and quantification of the analytes by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). All the variables involved in the extraction procedure have been accurately studied and optimized. The analytes were detected and quantified using a triple quadrupole mass spectrometer (QqQ). The selection of two specific fragmentation transitions for each compound allowed simultaneous quantification and identification. The method has been analytically characterized on the basis of its linearity, sensitivity and precision. Limits of detection ranged from 0.1 to 0.2ngmL(-1) with precision better than 8%, (expressed as relative standard deviation). Relative recoveries were in the range from 91 to 106% which demonstrated the applicability of the stir-membrane solid-liquid-liquid microextraction for the proposed analytical problem. Moreover, the method has been satisfactorily applied for the determination of parabens in lyophilized breast milk samples from 10 randomly selected individuals.
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
authors.forename: Rocío
authors.initials: R
authors.lastname: Rodríguez-Gómez
authors.affiliation: Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
authors.forename: Mercedes
authors.initials: M
authors.lastname: Roldán-Pijuán
authors.affiliation: Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
authors.forename: Rafael
authors.initials: R
authors.lastname: Lucena
authors.affiliation: Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
authors.forename: Soledad
authors.initials: S
authors.lastname: Cárdenas
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
authors.forename: Alberto
authors.initials: A
authors.lastname: Zafra-Gómez
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
authors.forename: Oscar
authors.initials: O
authors.lastname: Ballesteros
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
authors.forename: Alberto
authors.initials: A
authors.lastname: Navalón
authors.affiliation: Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain. Electronic address: qa1meobj@uco.es.
authors.forename: Miguel
authors.initials: M
authors.lastname: Valcárcel
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D059627:Liquid Phase Microextraction / Q000379:methods*; D008895:Milk, Human / Q000737:chemistry*; D052617:Solid Phase Microextraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D012997:Solvents
keywords: Lyophilized human milk samples; Parabens; Stir-membrane solid–liquid–liquid microextraction; UHPLC-MS/MS