色谱

色谱 ›› 2018, Vol. 36 ›› Issue (8): 795-802.DOI: 10.3724/SP.J.1123.2018.02022

• 研究论文 • 上一篇    下一篇

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

曲栗1,2, 曾静1, 赵超敏1, 宋伟民2   

  1. 1. 上海出入境检验检疫局, 上海 200135;
    2. 复旦大学公共卫生学院, 上海 200032
  • 收稿日期:2018-03-08 出版日期:2018-08-08 发布日期:2014-06-28
  • 通讯作者: 曲栗,Tel:+86-21-38620528,E-mail:qul@shciq.gov.cn
  • 基金资助:

    Technology Project of the Shanghai Inspection and Quarantine Bureau (No.HK009-2017);Science and Technology Joint Project of the Yangzte River Delta (No.17395810102).

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

QU Li1,2, ZENG Jing1, ZHAO Chaomin1, SONG Weimin2   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. School of Public Health, Fudan University, Shanghai 200032, China
  • Received:2018-03-08 Online:2018-08-08 Published:2014-06-28
  • Supported by:

    Technology Project of the Shanghai Inspection and Quarantine Bureau (No.HK009-2017);Science and Technology Joint Project of the Yangzte River Delta (No.17395810102).

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摘要：

建立了固相萃取-气相色谱-质谱法同时测定进口海产品中11种合成麝香（开司米木、萨利麝香、粉檀麝香、葵子麝香、特斯拉、佳乐麝香、二甲苯麝香、吐纳麝香、伞花麝香、西藏麝香和麝香酮）。样品经正己烷提取，弗罗里硅土固相萃取柱净化，内标法定量。目标物在0.001~0.1 mg/L内呈良好的线性相关，相关系数（r2）均大于0.990，方法检出限（信噪比（S/N）>3）为0.35~2.08μg/kg，定量限（S/N>10）为1.18~5.00μg/kg。分别在空白基质中添加低、中、高3个水平的标准品进行回收试验，平均回收率为83.1%~117%，相对标准偏差（RSD，n=6）为5.1%~8.5%。利用该方法对2017年上海口岸进口的30个海产品进行了筛查，发现佳乐麝香在93.3%的被测样品中均有检出，含量最高达3.82μg/kg。葵子麝香和伞花麝香也是检出较多的麝香品种，含量最高分别可达15.4μg/kg和10.5μg/kg。该方法特异性强，灵敏度高，适用于海产品中多种合成麝香残留物的筛查和确证。

关键词: 固相萃取, 合成麝香, 进口海产品, 气相色谱-质谱

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 n-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 (S/N>3) ranged from 0.35 to 2.08 μg/kg, and the limits of quantification (S/N>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.

Key words: gas chromatography-mass spectrometry (GC-MS), imported seafood, solid phase extraction (SPE), synthetic musks

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