高效液相色谱-串联质谱法测定牛奶和鸡肉中4种激素本底值
发布时间:2018-03-30 09:45
本文选题:激素 切入点:鸡肉 出处:《食品科学》2017年22期
【摘要】:建立牛奶和鸡肉中4种激素(睾酮、甲基睾酮、孕酮、氢化可的松)本底值同时测定的高效液相色谱-串联质谱方法。样品经β-葡萄糖醛酸酶/芳香基硫酸酯酶水解,加入乙腈超声提取,正己烷除脂肪。采用ZORBAX SB-C18色谱柱分离,以0.1%甲酸溶液和甲醇为流动相梯度洗脱,分别在电喷雾离子源正、负离子模式下以多反应监测模式分段扫描同时检测,基质匹配外标法定量。结果表明,4种激素在相应的质量浓度范围内线性良好,相关系数均大于0.991;在牛奶中的检出限(RSN=3)和定量限(RSN=10)分别为0.02~0.10μg/kg和0.06~0.33μg/kg,在鸡肉中的检出限和定量限分别为0.03~0.12μg/kg和0.10~0.40μg/kg;在3个水平下的平均回收率为牛奶56.0%~132.8%,鸡肉79.6%~122.0%;相对标准偏差为牛奶1.8%~17.3%,鸡肉2.0%~18.1%。该方法简单、快速、准确,适用于对牛奶和鸡肉中4种激素进行快速筛查和本底值测定。
[Abstract]:The samples were hydrolyzed by 尾 -glucuronidase / aromatic sulfate enzyme and extracted with acetonitrile.ZORBAX SB-C18 column was used to separate the samples, and 0.1% formic acid solution and methanol were used as mobile phase gradient elution. The results were detected simultaneously by multi-reaction monitoring mode in the mode of electrospray ion source and negative ion mode, respectively. The matrix matched external standard method was used to quantify the samples.The results showed that the four hormones were linear in the corresponding range of mass concentration.The difference is 1. 8 and 17. 3 and the chicken is 2. 0 and 18. 1.The method is simple, rapid and accurate. It is suitable for rapid screening and background determination of four hormones in milk and chicken.
【作者单位】: 中国检验检疫科学研究院食品安全研究所;内蒙古满洲里出入境检验检疫局技术中心;
【基金】:“十三五”国家重点研发计划重点专项(2016YFD0401103;2016YFF0203903)
【分类号】:O657.63;TS207.3
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