title: Rapid extraction and reverse phase-liquid chromatographic separation of mercury(II) and methylmercury in fish samples with inductively coupled plasma mass spectrometric detection applying oxygen addition into plasma.
abstract: A simple and sensitive procedure was developed for extraction and speciation of mercury in fish. Species separation was accomplished with reverse phase-high performance liquid chromatography (HPLC) hyphenated to inductively coupled plasma mass spectrometry (ICP-MS). Oxygen addition into plasma allowed use of organic-rich mobile phase, achieving species separation in 4 min. Mercury species extraction was achieved by microwave exposure for 2 min at mild conditions (60°C, pH 2.0), avoiding necessity of neutralizing sample prior to injection in HPLC, and reducing number of sample preparation steps, analytical source of errors and inter conversion of species. Limit of detection for entire procedure was found to be 0.2 and 0.1 ng g(-1) for mercuric ion and methylmercury, respectively. The method was applied to certified reference materials (TORT-2 and DORM-2) and commercialized fish samples (Mullus barbatus, Sparus aurata, Trachurus mediterraneus, Mugil soiuy, Dicentrarchus labrax, and Pomatomus saltatrix) from Black Sea.
authors: Çankırı Karatekin University, Faculty of Science, Department of Chemistry, 18100 Çankırı, Turkey. Electronic address: serchemist@gmail.com.
authors: Serhat
authors: S
authors: Döker
authors: Erciyes University, Faculty of Pharmacy, Department of Toxicology, 38039 Kayseri, Turkey. Electronic address: ipek4477@gmail.com.
authors: İffet İpek
authors: İİ
authors: Boşgelmez
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D005399:Fishes; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D008628:Mercury / Q000302:isolation & purification*; D008767:Methylmercury Compounds / Q000302:isolation & purification*; D008872:Microwaves; D010100:Oxygen / Q000737:chemistry; D013054:Spectrophotometry, Atomic
chemical_list: D008767:Methylmercury Compounds; D008628:Mercury; D010100:Oxygen
keywords: HPLC-ICP–MS; Marine fish; Mercury speciation; Methylmercury; Microwave assisted extraction