摘要
报道了一种同时筛选、定量和确证黄鳝中的11种性激素的灵敏、特异可靠的检测方法。对5.0 g肌肉样品,采用β-葡糖苷酸酶（来自Helix pomatia）对提取物水解后,经叔丁基甲醚提取,正己烷脱脂,再经C18小柱和NH2小柱净化,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1.00,2.50和5.00μg.kg-1,检出限在0.50～1.00μg.kg-1,平均回收率范围为56%～103%,平均相对标准偏差范围为3.1%～29.5%。对不同批次添加水平为1.00μg.kg-1的回收率进行比较,相对标准偏差范围为4.8%～22.2%,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非常有用。
A highly sensitive,specific and credible method for the simultaneous determination of 11 sex hormones in muscle of swamp eel is reported.Muscle tissues of swamp eel（5.00 g） were deconjugated by Helix pomatia juice,and extracted with tert-butyl methyl ether.After defatted by hexane,the extracts were cleaned-up through dual columns of C18 and NH2,and the extracts obtained were derivatized with heptafluorobutyric anhydride,following formation of the di-heptafluorobutyryl（di-HFB） derivative.Identification and quantification were carried out with capillary gas chromatography-mass spectrometry.External calibration was used for quantitation and the method was validated with blank samples（5 g each） fortified at 1.00,2.50 and 5.00 μg·kg-1.The detection limits were 0.50-1.00 μg·kg-1 for all analytes.Overall recovery and repeatability（relative standard deviations） and within-laboratory reproducibility ranged from 56% to 103%,and from 3.1% to 29.5%,respectively,for all analytes.The within laboratory repeatibility ranged from 4.8% to 22.2% when fortified at 1.00 μg·kg-1.The study showed that the recoveries and repeatability were good.Therefore,the method is useful for the animal food quality surveillance.
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第5期642-646,共5页
Journal of Instrumental Analysis
基金
国家质检总局资助项目<动物源性食品中多种性激素的测定>(2005IK033)
