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Determination of trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification-gas chromatography-mass spectrometry
Author(s) -
Liping Ding,
Chunping Cai,
Yi-Ting Lin,
WU Wen-fan,
Xiang Fang
Publication year - 2014
Publication title -
sepu/chinese journal of chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.171
H-Index - 19
eISSN - 1872-2059
pISSN - 1000-8713
DOI - 10.3724/sp.j.1123.2013.11025
Subject(s) - chemistry , chromatography , ketone , mass spectrometry , gas chromatography–mass spectrometry , bstfa , gas chromatography , extraction (chemistry) , selected ion monitoring , xylene , salting out , derivatization , toluene , organic chemistry , aqueous solution
In order to investigate the residues of musk xylene and musk ketone in aquatic products, a method was established for the determination of the trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification (MASP) -gas chromatography-mass spectrometry (GC-MS). After extracted with acetonitrile, the samples were pretreated using MASP method including extraction, salting-out and purification processes, analyzed with GC-MS in the selected ion monitoring (SIM) mode, and then quantified by matrix-matched standard solution in external standard method. The analysis was carried out with a capillary column (DB-5 MS, 30 m x 0.25 mm x 0.25 microm) under electron ionization conditions. The quantification was performed using monitoring ions of m/z 282, 297, 265 for musk xylene and m/z 279, 294, 191 for musk ketone. The results showed good linearity in the range of 1-100 microg/kg for musk xylene and musk ketone with the correlation coefficients not less than 0.999, and the limits of detection (S/N = 3) of 0.30 microg/kg. The average recoveries of musk xylene and musk ketone spiked in prawn, clam and sea eel blank samples at three spiked levels of 1.0, 2.0 and 10.0 microg/kg ranged from 79% to 104% and the RSDs were in the range of 1.6%-13.3%. The method is simple, rapid and accurate, and can be used for the routine analysis of musk xylene and musk ketone in aquatic products.

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