title: A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.
abstract: In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples.
authors.affiliation: School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangdong, Guangzhou 510275, China.
authors.forename: Xi
authors.initials: X
authors.lastname: Zhou
authors.affiliation: Instrumental Analysis and Research Center, Sun Yat-sen University, Guangdong, Guangzhou 510275, China.
authors.forename: Kunyan
authors.initials: K
authors.lastname: Cui
authors.affiliation: School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangdong, Guangzhou 510275, China. Electronic address: ceszf@mail.sysu.edu.cn.
authors.forename: Feng
authors.initials: F
authors.lastname: Zeng
authors.affiliation: School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangdong, Guangzhou 510275, China.
authors.forename: Shoucong
authors.initials: S
authors.lastname: Li
authors.affiliation: School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangdong, Guangzhou 510275, China.
authors.forename: Zunxiang
authors.initials: Z
authors.lastname: Zeng
mesh_terms: D015415:Biomarkers / Q000032:analysis; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D059625:Liquid-Liquid Extraction; D010795:Phthalic Acids / Q000032:analysis*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014465:Ultrasonics; D014675:Vegetables / Q000737:chemistry*
chemical_list: D015415:Biomarkers; D010795:Phthalic Acids; C032279:phthalic acid
keywords: High pressure liquid chromatography–electrospray ionisation-tandem mass spectrometry; Liquid–liquid extraction; Phthalate monoester metabolites; Solid-phase extraction; Ultrasonic extraction; Vegetable