摘要
建立了用安捷论GC-MS5975对黄鳝肌肉中20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5.0g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,异辛烷脱脂,经脱脂棉过滤后进入C18小柱,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5μg/kg,追宝龙按相应水平的5倍添加,以S/N≥3,甲睾酮、去氢睾酮和甲孕酮,检出限为0.25μg/kg,除了追宝龙的检测限为5μg/kg外,其他的检出限均为0.5~1μg/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11.6%~17.9%。当添加水平为1μg/kg(追宝龙为结果5μg/kg),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。
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 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 carded 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 5μ g/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.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2008年第6期298-303,共6页
Food Science
基金
国家质检总局资助项目(2005IK033)