Determination of trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification-gas chromatography-mass spectrometry

doi:10.3724/SP.J.1123.2013.11025

Abstract

Abstract:

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×0.25 mm×0.25 μm) 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 μg/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 μg/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 μg/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.

Key words: aquatic products, gas chromatography-mass spectrometry (GC-MS), multiple adsorption synchronous purification (MASP), musk ketone, musk xylene

CLC Number:

O658

DING Liping, CAI Chunping, LIN Yonghui, WU Wenfan, FANG Xiang. Determination of trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2014, 32(3): 309-313.

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