摘要
随着生活水平的提高,乳制品已是人们生活中不可缺少的一部分。乳制品中的性激素类兴奋剂残留的检测和判定,近年来已成为国内外广泛关注的一个热点。本研究在运用农业部标准方法的同时,对其样品前处理方法中存在的缺陷进行了改进,优化并选择了质谱分析的仪器条件,尤其是锥孔电压和碰撞能量的选择,建立了同时测定乳制品中7种性激素的超高压液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经过匀浆,乙腈和乙酸乙酯提取,固相萃取柱净化,液相色谱-电喷雾串联四极杆质谱,正离子多反应监测(MRM)模式进行测定。采用BEHC18色谱柱,以含0.1%甲酸的水和乙腈为流动相进行梯度洗脱。实验结果表明,7种性激素的方法检测限为0.2～0.4μg/kg,基质加标回收率为65～72%,相对标准偏差为12.5～24.2%。实际样品的分析表明,该法可实现对样品进行快速、灵敏、准确的定性定量分析,尤其适合于脂肪和蛋白含量较高的含乳制品。
As the improvement of people's living quality,milky products have become a necessary consumable.Sex hormones presented in milk products has become a problem of public concerned due to its potentially negative effect to human beings.Discrimination and determination of these hormones is the subject of residue analysis and control.The standard method suggested by China Department of Agricultural Ministry was adopted and some drawbacks were improved in this study.The instrumental conditions of LC-MS/MS were optimized,especially for the cone voltages and the collusion energy.A comprehensive analytical method based on ultra performance liquid chromatography-electrospray tandem mass spectrometry with passive mode and multiple reaction monitoring(MRM)has been developed for the simultaneous determination of 7 sex hormones residues in biological samples.The separation was performed on a Waters BEH C18 column with gradient elution using acetonitrile and water(containing 0.1 % formic acid).The method detection levels limits for the above 7 hormones were in the range of 0.2～0.4 μg/kg,the mean recoveries of matrix spiked samples were within 65 %～72 %,and the relative standard deviations were within 12.5 %~24.2 %.The real sample tests showed this method can be used for the fast,sensitive,and accurate determination of sex hormones residues in biological samples,especially for the milk and milk products.
出处
《食品安全质量检测学报》
CAS
2010年第1期36-42,共7页
Journal of Food Safety and Quality
基金
国家质检总局执法打假基金
关键词
性激素
兴奋剂
液相色谱-质谱
加标回收率
固相萃取
sex hormones
doping
liquid chromatography-mass spectrometry
recoveries
solid phase extraction
