FOOD SCIENCE ›› 2008, Vol. 29 ›› Issue (6): 298-303.

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Stimultaneous Determination of Residue of Sex Hormones in Eel Muscle by Gas Chromatography-Mass Spectrometry

 ZHAN  Jia, YU  Xue-Jun, LI  Zuo-Qing, XIE  Dong-Hua, FAN  Yuan-Mu, CHEN  Shu-Bing   

  1. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China
  • Online:2008-06-15 Published:2011-08-26

Abstract: A highly sensitive, specific and credible method for the simultaneous determination of 20 sex hormones in muscle of swamp eel performed by GC-MS(Agilent 5975) was studied.Muscle tissues of swamp eel (5.0 g) were hydrolyzed by glucuronidase from Helix pomatia juice, extracted by tert-butyl methyl ether, defatted by iso-octane, and cleaned-up through dual columns of C18 and NH2. The extracts obtained were derivatized with heptafluorobutyric anhydride, following formation of the di-heptafluorobutyryl (di-HFB) derivative, and then identification and quantification were carried out by means of capillary gas chromatography-mass spectrometry. For quantitation, the external standards were used and the method was validated with blank samples fortified at 1, 2.5 and 5 μg/kg with 5.0 g sample(trenbolone spiked 5 times as others). Results showed that the detection limits are 0.25~5μg/kg for all analytes. Average recovery (%) and coefficient of variance range from79.8% to 106.3%, and from 11.6% to 17.9%, respectively. The relative standard deviation (RSD) ranges from 9.3% to 22.1% at 1 mg/kg spiked level. The study results showed that the recovery and repeatability are good. Therefore, the method is very useful for the animal food quality surveillance at present.

Key words: sex hormone, GC-MS, swamp eel