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固相萃取-气相色谱-质谱法测定进口海产品中11种合成麝香

[Determination of 11 synthetic musks in imported seafood by solid phase extraction and gas chromatography-mass spectrometry].

作者信息

Qu Li, Zeng Jing, Zhao Chaomin, Song Weimin

机构信息

Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.

School of Public Health, Fudan University, Shanghai 200032, China.

出版信息

Se Pu. 2018 Aug 8;36(8):795-802. doi: 10.3724/SP.J.1123.2018.02022.

Abstract

A method has been developed for the simultaneous determination of 11 synthetic musks (cashmeran, celestolide, phantolide, musk ambrette, traseolide, galaxolide, musk xylene, tonalide, musk moskene, musk tibetene, and musk ketone) in imported seafood. The method combines solid phase extraction and gas chromatography-mass spectrometry. Samples were extracted by -hexane and purified using a Florisil column. Internal standards were used to correct for matrix effects. The calibration curves showed good linearity with correlation coefficients greater than 0.99. The limits of detection (>3) ranged from 0.35 to 2.08 μg/kg, and the limits of quantification (>10) were between 1.18 and 5.00 μg/kg. The average recoveries measured at three spiked levels (10, 20, and 30 μg/kg) were in the range 83.1%-117%, with relative standard deviations ranging from 5.1% to 8.5%. Further, the concentrations of 11 synthetic musks in 30 imported seafood in Shanghai were investigated. Galaxolide was detected in 93.3% of samples analysed, in concentration as high as 3.82 μg/kg. Musk ambrette and musk moskene were found in concentrations as high as 15.4 μg/kg and 10.5 μg/kg, respectively. The established method demonstrates high sensitivity and selectivity for the determination and confirmation of 11 synthetic musks in imported seafood.

摘要

已开发出一种同时测定进口海产品中11种合成麝香(佳乐麝香、天芥菜精、吐纳麝香、葵子麝香、异环麝香、新铃兰醛、二甲苯麝香、AHTN、西藏麝香、麝香酮)的方法。该方法结合了固相萃取和气相色谱 - 质谱联用技术。样品用正己烷萃取,并用弗罗里硅土柱净化。使用内标校正基质效应。校准曲线显示出良好的线性,相关系数大于0.99。检测限(>3)范围为0.35至2.08μg/kg,定量限(>10)在1.18至5.00μg/kg之间。在三个加标水平(10、20和30μg/kg)下测得的平均回收率在83.1% - 117%范围内,相对标准偏差在5.1%至8.5%之间。此外,还对上海30种进口海产品中11种合成麝香的含量进行了调查。在所分析的样品中,93.3%检测到新铃兰醛,浓度高达3.82μg/kg。葵子麝香和西藏麝香的浓度分别高达15.4μg/kg和10.5μg/kg。所建立的方法在测定和确证进口海产品中11种合成麝香方面显示出高灵敏度和选择性。

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