超高效液相色谱-串联质谱法测定牛奶中4,4'-硫代二苯酚残留量
Determination of 4,4'-dihydroxydiphenyl sulfide residues in milk by ultra-high performance liquid chromatography-tandem mass spectrometry
徐坤 1赵丰华 2刘霄飞 2杨修镇 2薄永恒2
作者信息
- 1. 山东省胶州市农业农村局,山东胶州 266300
- 2. 山东省畜产品质量安全中心,山东济南 250100
- 折叠
摘要
建立牛奶中4,4'-硫代二苯酚残留量的超高效液相色谱-串联质谱检测方法.用乙腈将牛奶中4,4'-硫代二苯酚全部提取,加入氯化钠去除脂类物质,用固相萃取柱去除杂质,采用超高效液相色谱-串联质谱仪检测4,4'-硫代二苯酚,以外标的方式进行定量.结果显示,4,4'-硫代二苯酚标准品的质量浓度在1.0～20.0 ng/mL范围内线性关系良好,相关系数r大于0.99.样品中4,4'-硫代二苯酚的检出限为0.5 μg/kg,定量限为1.0 μg/kg.在空白牛奶中添加4,4'-硫代二苯酚,质量浓度在1.0～5.0 μg/kg范围内,回收率均在60%～90%之间,计算得出相对标准偏差(RSD)均小于10%.该方法具有检测限低、回收率高、定性准确等优点,适用于牛奶中4,4'-硫代二苯酚残留量的检测.
Abstract
Ultra-high performance liquid chromatography-tandem mass spectrometry method and optimized conditions for the determination of 4,4'-dihydroxydiphenyl residues in milk were established.Milk samples were extracted with acetonitrile,defatted with sodium chloride,and purified with solid-phase extraction column.Quantification of the analyte was achieved by high performance liquid chromatography-mass spectroscopy using external standard.The results indicated that the correlations were greater than 0.99 at the range of 1.0 to 20.0 ng/mL.The limit of detection of 4,4'-dihydroxydiphenyl was 0.5 μg/kg,and the limit of quantification was 1.0 μg/kg.The average recoveries of 4,4'-dihydroxydiphenyl ranged from 60%to 90%at spiled levels of 1.0 to 5.0 μg/kg with RSD less than 10%.The experiment show that the method presents low detection limit,high recovery,qualitative standard for detection of 4,4'-dihydroxydiphenyl residues in milk.
关键词
牛奶/4,4'-硫代二苯酚/残留量/超高效液相色谱-串联质谱法Key words
milk/4,4'-dihydroxydiphenyl/residue/ultra-high performance liquid chromatography-tandem mass spectrometry引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据