摘要
目的建立猪肉中15种糖皮质激素残留的定性定量分析方法。方法采用固相萃取技术处理样品,通过高效液相色谱-四极杆-飞行时间质谱（HPLC-Q-TOF-MS）对猪肉中的15种糖皮质激素进行分离和检测,通过考察方法检测限、精密度、回收率等指标对方法学进行验证。建立糖皮质激素的精确相对分子质量数据库,并通过碎片离子的精确质量数推测碎片结构。结果 15种目标化合物检测限为0.1～1μg/kg,化合物回收率在47.1%～110.3%之间,精密度在3.9%～19.0%（n=6）之间。建立了共15种糖皮质激素的精确相对分子质量数据库。结论建立的方法准确、快速、灵敏度高,结合精确相对分子质量数据库,可对猪肉中糖皮质激素残留进行快速分析。
Objective To establish a novel analytical method to analyze 15 glucocorticoids residues in pork by high performance liquid chromatography-Q-time of fight mass spectrometry.Methods The analytes were extracted from the samples with acetonitrile and water.After cleaned up with C18 SPE column,samples were analyzed by HPLC-Q-TOF-MS with an electrospray interface in positive ionisation mode.The validation of the method consisted of limit of detection（LOD）,limit of quantification（LOQ）,precision and recovery.The accurate mass database was established and the accurate mass of characteristic fragments indicated the structures of the fragments.Results The LODs for 15 validated compounds were 0.1-1 μg/kg,and the average recoveries were in the range of 47.1%-110.3% with the relative standard deviations（RSD） 〈20%（n = 6）.Conclusion The results indicated that this method was simple,rapid,sensitive and suitable for the determination of glucocorticoids in pork.
出处
《中国食品卫生杂志》
2016年第2期204-208,共5页
Chinese Journal of Food Hygiene
关键词
高效液相色谱
飞行时间质谱
糖皮质激素
猪肉
兽药残留
食品安全
High performance liquid chromatography
time of flight mass spectrometry
glucocorticoids residues
pork
residue of veterinary drug
food safety
