色谱

色谱 ›› 2013, Vol. 31 ›› Issue (5): 485-489.DOI: 10.3724/SP.J.1123.2012.11017

• 技术与应用 • 上一篇    下一篇

分散固相萃取-气相色谱-质谱联用法测定水产品中的痕量酮麝香

丁立平*, 郭菁, 陈志涛, 赵建晖, 郑铃, 蔡伟   

  1. 福清出入境检验检疫局技术中心, 福建 福清 350300
  • 收稿日期:2012-11-26 修回日期:2013-01-14 出版日期:2013-05-28 发布日期:2013-05-16
  • 通讯作者: 丁立平,Tel:(0591)62837267,E-mail:43548624@qq.com.
  • 基金资助:

    福建出入境检验检疫局科技项目(FK2012-16).

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

DING Liping*, GUO Jing, CHEN Zhitao, ZHAO Jianhui, ZHENG Ling, CAI Wei   

  1. Technology Center of Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China
  • Received:2012-11-26 Revised:2013-01-14 Online:2013-05-28 Published:2013-05-16

PDF

338

被引次数

1

摘要：

建立了水产品中痕量酮麝香测定的分散固相萃取-气相色谱-质谱联用法(GC-MS)。目标化合物经1%乙酸-乙腈高速匀浆提取,以N-丙基乙二胺(PSA)、C18和石墨化碳(GCB)混合物为分散剂对其进行净化,采用GC-MS在选择离子监测模式下测定,外标法定量,并应用正交试验对前处理条件进行优化,以及对酮麝香的裂解机制进行探讨。在优化条件下,方法在1～50 μg/L范围内线性关系良好,相关系数不低于0.999,检出限(S/N=3)为0.30 μg/kg。对于明虾和罗非鱼空白样品,在1.0、2.0、10.0 μg/kg 3个水平下的加标回收率为91.8%～110.6%,相对标准偏差(RSD)为2.6%～8.4%。该方法操作简便、快速、准确,可用于水产品中痕量酮麝香的日常检验。

关键词: 分散固相萃取, 气相色谱-质谱法, 水产品, 酮麝香

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

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