Determination of musk ketone in aquatic products by gas chromatography-mass spectrometry with dispersive solid phase extraction

doi:10.3724/SP.J.1123.2012.11017

Abstract

Abstract:

A dispersive solid phase extraction coupled with gas chromatography-mass spectrometry (GC-MS) method was established for the determination of trace amounts of musk ketone in aquatic products. The target analyte in the samples was extracted with acetonitrile containing 1% acetic acid, cleaned-up with the mixture of N-propyl-ethylenediamine (PSA), C₁₈ and graphitized carbon (GCB), and analyzed by GC-MS under selected ion monitoring (SIM) mode and quantified by the external standard method. The orthogonal experiment was carried out to optimize the pre-treatment conditions. Under the optimal conditions, good linear relationship was obtained in the range of 1-50 μg/L for musk ketone with correlation coefficient not less than 0.999, and the limits of detection (S/N=3) was 0.30 μg/kg. The recoveries of musk ketone in the prawn and tilapia blank samples at three spiked levels of 1.0, 2.0 and 10.0 μg/kg ranged from 91.8% to 110.6% with RSDs in the range of 2.6%-8.4%. The method is simple, rapid and accurate, and can be used for the routine analysis of musk ketone in aquatic products.

Key words: aquatic products, dispersive solid phase extraction, gas chromatography-mass spectrometry (GC-MS), musk ketone

CLC Number:

O658

DING Liping, GUO Jing, CHEN Zhitao, ZHAO Jianhui, ZHENG Ling, CAI Wei. Determination of musk ketone in aquatic products by gas chromatography-mass spectrometry with dispersive solid phase extraction[J]. Chinese Journal of Chromatography, 2013, 31(5): 485-489.

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