色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法检测动物肌肉组织中残留的甾类同化激素

陈捷,秦燕,张美金

  

  1. Food Inspection Center, Guangzhou Entry & Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • 收稿日期:2005-02-21 修回日期:2005-11-21 出版日期:2006-01-30 发布日期:1987-09-25
  • 通讯作者: 陈捷

Determination of Anabolic Steroid Hormones in Animal Muscle Tissues by Gas Chromatography/Mass Spectrometry

CHEN Jie, QIN Yan, ZHANG Meijin   

  1. Food Inspection Center, Guangzhou Entry & Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • Received:2005-02-21 Revised:2005-11-21 Online:2006-01-30 Published:1987-09-25

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摘要：

建立了不同动物肌肉中甾类同化激素残留的气相色谱/质谱（GC/MS）检测方法。样品经酶解、组织捣碎和超声提取后,用叔丁基甲醚萃取和反相固相萃取柱净化,进一步衍生后进行GC/MS分析，分别测定雄激素（表睾酮（ETS）、丙酸睾酮（PTS）、19-去甲基睾酮（17β-NT）、甲基睾酮（MTS）)和雌激素（雌二醇（17β-ES）、雌三醇（EST）、炔雌醇（EES）、雌酮（ESN）、苯甲酸雌二醇（BES)）。实验结果表明，ETS、17β-NT、MTS、PTS、BES、ESN、17β-ES、EES和EST的定量检测限为1.0~2.0 μg/kg。在2.0 μg/kg的定量检测低限添加水平,上述9种激素的平均回收率为62.5%~80.5%,相对标准偏差为12.5%~26.8%。该法可实现对样品进行灵敏、准确的定性定量分析。

关键词: 多残留分析 , 固相萃取, 气相色谱/质谱联用, 甾类同化激素

Abstract:

A gas chromatography/mass spectrometry (GC/MS) method was developed for the determination of multi-residues of steroid anabolic hormones epitestosterone (ETS), testosterone 17-propionate (PTS), nandrolone (17β-NT ), 17α-methyltestosterone (MTS), 17β-estradiol (17β-ES),estriol(EST), 17α-ethinylestradiol (EES), estrone (ESN) and 17β-estradiol 3-benzoate (BES) in the muscle tissues of various animal species. Homogenized tissue samples were enzymatically digested in acetate buffer (pH 5.0). Consequently, methanol was added and the mixtures were extracted under ultrasonication incubation. Clean-up was carried out for at least two times with methyl tert-butyl ether (MTBE) liquid-liquid partitioning followed by a reversed-phase solid phase extraction (SPE) cartridge purification. The eluate with methanol was evaporated to dryness by N2 at 40 ℃ and derivatization was achieved with N-methyl-N-(trimethylsilyl) trifluoroacetamide/iodotrimethylsilane/dithioerythritol （MSTFA-TMIS-DTE） at 60 ℃ for 45 min. The reaction mixture was injected into a gas chromatograph with a DB-1 capillary column coupled with a mass spectrometer . The samples were tested by different selected ion monitoring modes with electron impact （EI） source for the androgens and estrogens. The limits of quantitation (LOQ) for the above 9 hormones were in the range of 1.0-2.0 μg/kg. At the 2.0 μg/kg LOQ spiked level, the mean recoveries were within 62.5%-80.5%, and the relative standard deviations were within 12.5%-26.8%. The real sample tests showed this method can be used for the sensitive and accurate determination of multi-steroid anabolic hormones residues in biological muscle samples.

Key words: anabolic steroid hormones, gas chromatography/mass spectrometry (GC/MS), multi-residue analysis
, solid phase extraction