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Comparison of different derivatization approaches for mercury speciation in biological tissues by gas chromatography/inductively coupled plasma mass spectrometry
Author(s) -
García Fernández Rubén,
Montes Bayón María,
García Alonso J. Ignacio,
SanzMedel Alfredo
Publication year - 2000
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/(sici)1096-9888(200005)35:5<639::aid-jms990>3.0.co;2-g
Subject(s) - chemistry , derivatization , certified reference materials , inductively coupled plasma mass spectrometry , mercury (programming language) , chromatography , methylmercury , gas chromatography , gas chromatography–mass spectrometry , reagent , mass spectrometry , detection limit , aqueous solution , standard addition , sample preparation , environmental chemistry , organic chemistry , bioaccumulation , computer science , programming language
Abstract A novel interface design for coupling gas chromatography and inductively coupled plasma mass spectrometry (GC/ICP‐MS) was used to perform mercury speciation in biological tissues. Three derivatization approaches were optimized and compared for this purpose: anhydrous butylation using a Grignard reagent, aqueous ethylation by means of NaEt 4 B and aqueous propylation with NaPr 4 B. The last reagent was synthesized in the laboratory as it is not commercially available. Detection limits obtained by GC/ICP‐MS ranged between 100 and 200 fg (as absolute mass) for methylmercury and between 500 and 600 fg for inorganic mercury using a 1 µl injection. Quantification of methyl‐ and inorganic mercury was carried out by resorting to aqueous calibration, using ethylmercury as internal standard for both propylation and butylation derivatization techniques. For ethylation procedures, a methylpropylmercury solution was used as internal standard. The absence of transmethylation during sample preparation was checked using a 97% enriched 202 Hg inorganic standard. The accuracy of the three derivatization approaches was evaluated by the analysis of the certified reference material DOLT‐2 (dogfish liver) from the National Research Council of Canada and certified for methylmercury, with satisfactory results. Copyright © 2000 John Wiley & Sons, Ltd.