1. 上海出入境检验检疫局
2. 中国检验检疫科学研究院
3. 烟台出入境检验检疫局
4. 天津出入境检验检疫局
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王敏, 张秀芹, 杨振宇, 等. HPLC-MS/MS检测含蛋白质辐照食品中的邻酪氨酸[J]. 分析测试学报, 2011,30(10):1187-1190.
Determination of o-Tyrosine in γ-Ray Irradiated Protein-rich Food by HPLC-MS/MS[J]. 2011,30(10):1187-1190.
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,deproteinated 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.
邻酪氨酸含蛋白质辐照食品液相色谱-串联质谱
o-tyrosineγ-ray irradiated protein-rich foodHPLC-MS/MS
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