摘要
应用液相色谱-串联质谱(HPLC-MS/MS)技术建立了含蛋白质辐照食品中邻酪氨酸的检测方法。样品经胰蛋白酶于37℃水解过夜,正己烷去脂,乙酸锌沉淀蛋白净化后,HPLC-MS/MS检测。方法的定量下限为0.1 mg/kg,邻酪氨酸在0.1、0.5、1.0 mg/kg加标水平的回收率为80%～97%,相对标准偏差(RSD,n=6)为6.3%～12.9%。在2.0、5.0、10 kGy 3个辐照剂量水平下,鸡肉、猪肉、牛肉、鱼肉和虾肉中的邻酪氨酸含量为0.095～0.677 mg/kg,邻酪氨酸含量与辐照剂量呈线性相关,相关系数(r)大于0.98。该方法灵敏、实用性强。
A liquid chromatography - tandem mass spectrometric method was developed for the determination of o-tyrosine in γ-ray irradiated protein-rich food. The sample was homogenized and hydrolyzed with parenzyme at 37 ℃ for 24 h. The digestion solution was purified with n-hexane eliminating fat, dcproteinated with zinc acetic acid solution, and then determined by HPLC -MS/MS. The quantitation limit was 0. 1 mg/kg. The recoveries of o-tyrosine at three spiked levels of 0. 1, 0.5 and 1.0 mg/kg were in the range of 80% - 97% with RSDs（n =6） of 6.3% - 12.9% . The o-tyrosine contents in chicken, pork, beef, fish and shrimp irradiated with 2, 5, 10 kGy of γ-ray ranged from 0. 095 mg/kg to 0. 677 mg/kg, which were obviously higher than those in the unirradiated meat samples, and presented linear relationships with the irradiance dose. The method showed good reproducibility and sensitivity.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第10期1187-1190,共4页
Journal of Instrumental Analysis
基金
质检公益性行业科研专项项目(200910142)
