黄鳝肌肉中的20种性激素同时测定的气质联用检测方法.pdfVIP

298 2008,Vo1．29，No．06 食品科学 ※分析检测 黄鳝肌肉中的2 0种性激素同时 测定的气质联用检测方法 湛 嘉，俞雪钧，李佐卿 ，谢东华，樊苑牧，陈树兵 (宁波出入境检验检疫局，浙江 宁波 315012) 摘 要：建立了用安捷论GC—MS5975对黄鳝肌肉中2O种性激素能同时进行筛选、定量和确证的灵敏、特异可靠 的检测方法。对5．Og肌肉样品，采用p一葡糖苷酸酶(来自Helix pomatia)对提取物水解后，经叔丁基甲醚提取，异 辛烷脱脂，经脱脂棉过滤后进入C s小拄，再经NH2小柱净化后七氟丁酸酐对其进行衍生，最后利用GC—MS进行 检测。采用外标法定量，通过对空白样品添加标准品，使之理论含量为1、2．5和511g／kg，追宗龙按相应水平的 5倍添加，以S／N≥3，甲睾酮、去氧睾酮和甲孕酮，检出限为0．2511g／kg，除了追宅龙的检测限为511g／kg外，其 他的检出限均为0．5～111g／kg。对待测物三个水平的添加回收实验表明，平均回收率范围为79．8％～106．3％，平均 变异系数的范围为l1．6％～17．9％。当添加水平为llaglkg(追宝龙为结果5laglkg)，本方法不同批次回收率的相对偏差 范围为9．3％～22．1％，重复性好。因此，本方法对目前动物源食品中的性激素监督检验有参考价值。 关键词：性激素；气相色谱一质谱联用；黄鳝 · Sfimultaneous 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 (Ningbo Entry—Exit Inspection and Quarantine Bureau，Ningbo 3 15012，China) 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 Helixpomatia jtfice，extracted by tert-butyl methyl ether，defatted by iso-octane，and cleaned—up through dual columns of Cl8 and NH2．The extracts obtained were derivatized with heptafluorobutyric anhydride．following form ation of the di—heptafluorobutyryl(di—HFB)derivative，and then identification and quantification were carded out by means of capillary gas chromatography—mass spectrometry．For quantitation，the external standards were used and the method was validated with blank samplesfortified at 1．2．5 and 5u g／kgwith 5．0g sample(trenbolone spiked 5times aS o